UNDERGRADUATE THESIS PROJECT PROPOSAL

Department of Chemical Engineering

De La Salle University – Manila

Efficiency of Carbon Capture by Aqueous Ammonia

from Combustion of Semirara Industrial Grade Sub-bituminous Coal

Submitted by:

Stephanie Jane P. Siy

Chemical Engineering Minor in Semiconductor Processing

Janina Charisse Villanueva

Chemical Engineering

Alexis Pulhin
Chemical Engineering

MERECHE
Section EA1 (8 a.m.)
November 30, 2010

Thesis Adviser: PhD. Susan A. Roces

Thesis Co-Adviser: PhD. Nathaniel P. Dugos

On my honor as a University student, on this assignment I have neither given nor

received unauthorized aid as defined by the Guidelines on Academic Honesty
of the Student Handbook.
Signed ___________________________________
 Table of Contents

List of Tables.................................................................................................................................................i

List of Figures...............................................................................................................................................ii

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

1.1 Background of the Study...................................................................................................1

1.2 Problem Statement............................................................................................................1
1.3 Objectives..........................................................................................................................2
1.3.1 General Objectives.....................................................................................................2
1.3.2 Specific Objectives....................................................................................................2
1.4 Significance of the Study..................................................................................................2
1.5 Scope and Limitations.......................................................................................................2
Chapter 2: Review of Related Literature.....................................................................................................4

2.1 Coal: Its General Properties and its Uses..........................................................................4

2.1.1 World Coal Consumption..........................................................................................4
2.1.2 Environmental Impacts of Coal Consumption and Implemented Regulations.........6
2.1.3 Coal Consumption and CO2 Emission in the Philippines..........................................7
2.1.4 Coal in the Philippines...............................................................................................7
2.1.5 Regulations implemented on Reducing CO2 Emissions in the Philippines...............8
2.2 Carbon Capture Technologies...........................................................................................9
2.2.1 Chemical Looping Combustion or Chemical Looping Reforming...........................9
2.2.2 Adsorption...............................................................................................................10
2.2.3 Absorption...............................................................................................................11
2.3 Incorporation of Ammonia in Decarbonisation Absorption...........................................14
Chapter 3: Theoretical Framework............................................................................................................16

3.1 Chemical Properties of Ammonia...................................................................................16

3.2 Reactions Involved in Ammonia Decarbonization.........................................................17
3.3 NH3-CO2 –H2O Equilibrium Diagram.............................................................................18
3.4 Absorption.......................................................................................................................18
3.4.1 Material balance.......................................................................................................18
3.4.2 Limiting Gas-Liquid Ratio......................................................................................19
3.4.3 Multicomponent Absorption....................................................................................19
3.5 Wetted-Wall Column......................................................................................................20
Chapter 4: Materials and Methodology.....................................................................................................21

4.1 Materials..........................................................................................................................21
4.2 Experimental Setup.........................................................................................................21
4.3 Experimental Procedures................................................................................................22
4.3.1 Combustion of Semirara Coal.................................................................................22
4.3.2 Preparation of Aqueous Ammonia Sample............................................................23
References.................................................................................................................................................24

Appendix...................................................................................................................................................29
A. Calculations.....................................................................................................................29
B. Materials Safety Data Sheet................................................................................................30
List of Tables

Chapter 2

Table 2.1 Updated coal consumption statistics (in thousand short tons)
of the world and top 40 countries as conducted
by the Energy Information Administration during the year 2008....................................................5

Table 2.2 Update coal CO2 emission statistics (in million metric tons)
of the world and top 40 countries as conducted by the
Energy Information Administration during the year 2008..............................................................6

Table 2.3 Industrial grade Semirara coal constituents

obtained from the Semirara Mining Corporation.............................................................................8

Chapter 3

Table 3.1 Physical properties of ammonia (NH3)

obtained from Perry’s Chemical Engineering Handbook..............................................................16

Table 3.2 Vapor pressure of ammonia (NH3) and corresponding temperature

as obtained from Perry’s Chemical Engineering Handbook..........................................................16

Table 3.3 List of equilibrium reactions involved

in ammonia absorption...................................................................................................................17

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List of Figures

Chapter 2

Figure 2.1 Rapid screening apparatus incorporated

in the methodologies of Aronu et al. and Ma’mun et al.
as obtained from Aronu et al. (2009).............................................................................................13

Figure 2.2 Schematic diagram of the procedures used by Puxty et al. (2010)
in determining the load capacities of ammonia and MEA.............................................................14

Chapter 3

Figure 3.1 Ternary diagram of NH3-CO2 –H2O system at 40˚C and 1 bar
as presented in UNIQUAC model.................................................................................................18

Figure 3.2 Overall volumetric mass transfer coefficient vs.

gas-liquid ratio (Qiu et al., 2010)...................................................................................................19

Chapter 4

Figure 4.1 Qian’s wetted-wall column design...............................................................................21

Figure 4.2 Experimental setup.......................................................................................................21

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 Chapter 1: Introduction

1.1 Background of the Study

As the world is experiencing the dilemmas brought about by global warming, scientist are
growing more aware about the consequences that result from technological advancement. As the
preservation of the stability of nature is deemed crucial at these times, various researches are
conducted to determine the sources that caused this and to find solutions that would prevent
further degradation of the environment. Recently, there devised methods of controlling, hiding
and, even highly recommended the total elimination of greenhouse gases.

Researches were conducted in order to find the solution to this problem and thus lead to
the emergence of green technologies. However, due to economic and political means, coal and
fossil fuels still play a big role in generating energy in industrial sectors since it is made a
spectacle in the international market. Considering this situation, carbon dioxide capture is opted
as a means of preventing air pollution while the presence of said fuels is still abundant.

So far, methods involved in sequestration of carbon dioxide can be applied before (pre-
combustion) or after (post-combustion). Among the said methods are membrane technology,
adsorption, absorption, cryogenics, carbon extraction, biotechnology (cyanobacteria) and energy
conversion (Feron & Hendriks, 2005). Just recently, among these also include the new carbon
capture methods namely chemical looping cycle (CLC) which involves the transfer of oxygen
with both the gas and fuel separated (Yang et al., 2008) and chemical looping reforming (CLR)
which are done whilst producing synthesis gas (Rydén, Lyngfelt, & Mattisson, 2006). Efficiency
of each method will depend on the different parameters applied on the medium, kinds of fuel and
the properties of the flue gas produced before, during or after combustion.

CO2 capture and storage (CCS) is currently available for large companies that produce
large emissions(Kirchsteiger, 2008). Although promising as it sounds, applying it at a global
scale may yet be costly for most to afford. Furthermore, this method could potentially amount to
grave hazards. CCS involves storing the collected CO 2 underground and that requires transport
through pipes. In addition to that, there are uncertainties of situations that may arise from
accidental release of CO2 from pipe leaks and what’s worse is that effects may reach
globally(Kirchsteiger, 2008). Moreover, the fact that the CO 2 gas does not undergo any
significant reaction would only lead to its accumulation over the years (Kirchsteiger, 2008). But
since solutions are called for at a sooner time, CCS may serve as an off-setter for the time being.

1.2 Problem Statement

In fulfilment of alleviating the effects of greenhouse gases and to increase awareness of

this issue, this paper shall disseminate information about one of the clean coal technologies that
can be used in third world countries such as the Philippines. One of which is what this paper
focuses on, carbon capture using aqueous ammonia.

Previous studies so far elucidate absorption capacities of aqueous ammonia through the
generation of artificial flue gas, thus this paper will involve the combustion of Semirara sub-

1
bituminous industrial grade coal to produce the flue gas for testing the absorption of aqueous
ammonia at different concentrations. Absorption of different aqueous ammonia concentrations
shall be determined through the material balance of input and output fluids. Comparison of gas
composition before and after absorption process will indicate the efficiency solvent given its
corresponding concentration.

1.3 Objectives

1.3.1 General Objectives

This paper aims to prove and evaluate the effectiveness of aqueous ammonia in absorbing
carbon dioxide from multi-component flue gas such as combustion products from coal.

1.3.2 Specific Objectives

1. Determine the percent conversion of coal fuel to flue gas by the analysis of the contents of
the following gases: CO2, CO, H2, O2, N2, H2O, and SO2.

2. Compute for the pressure of flue gas prior to achieving CO2 partial pressure of 20 kPa.

3. Obtain CO2 content before and after flue gas is made to pass through absorption column.

1.4 Significance of the Study

This main purpose of the study is to help in alleviating pollution and global warming. It
aims to discover ways to capture carbon efficiently and effectively. It is designed for lessening
carbon emissions (on a large scale) using processes and materials suitable for the Philippine
setting; low-cost, abundant, practical and economical techniques which may be easily available
to the country’s industries.

So far, studies had gone as far as using mixed CO2 and N2 in order to simulate the flue
gas. This time natural flue gas is used to simulate actual combustion of coal in power plants. A
small sample of Semirara coal shall be combusted to test the CO 2 absorption capacities of
aqueous ammonia in different concentrations. The amount of other fuel constituents such as
sulphur and hydrogen and their products shall be taken into account since they are absorbable as
well. This will determine whether prior processes have to be done to isolate CO 2 or CO2
absorption from mixed flue gas is efficient that additional process need not be added.

1.5 Scope and Limitations

The research shall cover the use of ammonium absorption decarbonisation technology in
the post combustion setting. Variables such as different concentrations of ammonia shall be used
against the combustion of Semirara industrial grade coal. Hence, absorption principles shall be
applied. To conform to the space provided by the laboratory, small amounts of samples (10
grams of coal and 10 grams of solvent) and a small scale design of the wet wall column of which
dimensions vary from existing literature will be utilized. Since other coal constituents will be

2
included as previously mentioned, analysis of the actual conversion of fuel into flue gas is
required before doing the analysis of the absorbent. Then after the production of flue gas from
combustion, absorption capacity shall be determined from the CO2 content and other absorbed
gas content from circulated solvent. The wet wall column shall be fabricated such that
dimensions that simply allow contact between solvent and solute. Also, temperature at the
absorption part will have to be maintained at 20˚C to prevent the vaporization of ammonia as
suggested by literature. Absorption will be indicated by the change of pressure, and through the
calculation of the mass fraction of flue gas components at the inlet and outlet.

Factors excluded in this research are the rate of absorption and the gas used for stripping
the absorbent of CO2 content for regeneration. Hence this might yet exclude the determination of
the mass transfer coefficient. Furthermore, preloading of CO 2 gas shall not be included in the
procedures.   
 

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 Chapter 2: Review of Related Literature

2.1 Coal: Its General Properties and its Uses

Coal is a carbon rich, combustible sedimentary rock that is formed from accumulated
fossilized remains of prehistoric colossal life forms, otherwise known as fossil fuel (National
Energy Education Development Project). Properties of coal such as their carbon content,
inorganic traces and calorific value may vary from the way fossil fuel coalifies. Quality of
coalification depends on the organic composition of the material, temperature and pressure
related to the depth of the coal’s burial, and the length of time it was left to coalify (World Coal
Association). In order to rank coal by its quality, coal is classified into four categories namely
anthracite, bituminous, sub-bituminous and lignite.

Coal mainly starts with peat which is usually an immature coal that is previously left to
coalify for more or less a million years (Roces, 2010). If given a few million more years, the coal
may become lignite which is characterized with a dark brown to black color. Lignite has a
calorific value of 4000 to 8300 Btu/lb and this is sufficient to provide energy for generating
electricity (Kentucky Educational Television). Then billion years more could gradually coalify
the once lignite into sub-bituminous, bituminous and then anthracite. Sub-bituminous coal’s
calorific value of 8300 to 13000 Btu/lb is considered to give a cleaner flue gas with its high
energy, while bituminous coal has a calorific value of 10000 to 15500 Btu/lb is highly favourable
enough to supply intense heat for metallurgic processes (Kentucky Educational Television).
Lastly, anthracite, the hardest coal yielding a calorific value of more or less 15000 Btu/lb m and is
rarely used in any operations but house heating, therefore lowering its demands in the market
(Kentucky Educational Television). The more immature coal contains more combined water.

Besides obtaining coal from mines that contain natural reserves of fossil fuels, coal can
also be processed manually. It is important to consider the impurities and non-organic traces that
would lower the energy value that coal produces. Therefore, the coal will have to be heated to
allow the polymerization of aromatics, releasing impurities and retaining the volatile carbon
content (Menendez & Alvarez).

2.1.1 World Coal Consumption

The following history is as stated by the National Energy Education Development

Project. Before coal was discovered by the European colonizers, coal was long used by
indigenous people such as the native North Americans. Upon the discovery of the European
colonizers, it was not given much significance until it became widely used in mass production
during the 1800’s. However during the 20th century the demand for coal began its decline as
there appeared an increased in demand for petroleum as America enters the “motorized” trend in
machinery (Smiley, 2010). It was at the 70’s when coal made a turning point, until its
consumption broke the average record until year 2008. Currently, it comprises 23% of the
America’s energy supply. Also, according to the latest statistics conducted by the World Coal
Association (2010) during 2008, China was the top producer of hard coal, Australia was the top
exporter of coal, while Japan was the top importer of coal.

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 Coal is widely used by the domestic and industrial sectors to provide energy in daily
operations. Being an abundant high energy source, given the fact that it also readily provides
energy in its raw form by being burned directly into combustion engines, coal was priced to be
one of the cheapest fuels since the 70’s. Another factor that contributed to its low market price
would be the expansion of coal markets which was once initiated by European countries and
colonies and the improvement of transnational transportation (Ellerman, 1995), therefore leading
to the lowering of transportation costs and then the price of oil.

The increasing demand made coal one of the bases of evaluating the GDP of countries
since this vein of black gold is what makes a country capable of circulating its economy through
the industries that rely on this energy and the exports that will yet supply other industries off-
coast. Also this requires tremendous amount of labor force to obtain it. Furthermore, coal has
reserves that could last for about 122 years which is longer compare to other fuel sources like oil
and gas, which are estimated to last for only about 42 and 60 years based on the current rate of
consumption (World Coal Institute, 2010). Reasons like these plus the demand for energy makes
coal an object of politics. Currently, the United States, being the residual supplier of coal, is the
one dictating the price of coal in the market.

Table 2.1 shows the coal consumption of some countries and the total world consumption
during the year 2008. According to the table, the world consumes a total of about 7.3 billion
short tons of coal.

Table 2.1 Updated coal consumption statistics (in thousand short tons)
of the world and top 40 countries as conducted by the
Energy Information Administration during the year 2008

3004414.6
1 China 5 21 Serbia 43805.85
1120548.4
2 United States 4 22 Thailand 38282.71
3 India 632357.45 23 Bulgaria 36385.09
4 Germany 267881.50 24 Korea, North 33161.93
5 Russia 249795.88 25 Spain 28553.17
6 Africa 227447.62 26 Italy 27203.94
7 Japan 203803.04 27 Brazil 24610.20
8 Australia 157896.18 28 Vietnam 24588.16
9 Poland 148914.55 29 France 21119.18
1
0 Korea, South 110522.15 30 Estonia 17415.42
1
1 Turkey 108836.71 31 Mexico 16709.94
1
2 Ukraine 78009.47 32 Israel 14257.30
1
3 Kazakhstan 75922.80 33 Netherlands 14061.08
1 Greece 71822.20 34 Philippines 13099.87

5
 4
1
5 Indonesia 71497.02 35 Hungary 12760.36
1
6 Taiwan 69396.03 36 Bosnia and Herzegovina 12697.52
1
7 United Kingdom 64506.16 37 Hong Kong 12505.68
1
8 Canada 61858.41 38 Pakistan 9249.49
1
9 Czech Republic 59851.10 39 Slovakia 8992.66
2
0 Romania 44472.75 40 Chile 8589.82
World 7345641.28

2.1.2 Environmental Impacts of Coal Consumption and Implemented Regulations

The increase consumption of fossil fuels amounted to an increase in the production of

greenhouse gases, which in effect led to global warming. The abrupt change in climate raised the
awareness of many nations and therefore began the search for alternatives and strategies to
prevent the total degradation of the environment. In comparison of the data in Table 2.1 and
Table 2.2 (which shows the emissions taken by the same source as that of the previous during the
same year) 7 billion short tons of coal during the year 2008 and in turn produced CO 2 emission
that amounted to over 12 billion metric tons. Also, the same top 40 countries appeared in both
tables with the first three having the same order of coal consumption and CO 2 emission.
Although the rest of the countries are not the same as that of the first three, it is clearly implied
that the increase of emission is dependent of the amount of coal burned.

Table 2.2 Update coal CO2 emission statistics (in million metric tons)
of the world and top 40 countries as conducted by the
Energy Information Administration during the year 2008

5381.9981
1 China 4 21 France 51.83643
2 United States 2125.1675 22 Brazil 50.69332
1025.5486
3 India 5 23 Spain 49.54101
4 Russia 447.70069 24 Netherlands 45.412
5 Japan 441.20269 25 Romania 41.0485
6 Germany 318.50847 26 Malaysia 35.98659
7 Korea, South 248.42308 27 Serbia 34.73217
8 Australia 239.02891 28 Greece 32.87302
9 Poland 204.02507 29 Hong Kong 32.17582
1
0 Indonesia 179.16124 30 Israel 31.72546
1 Taiwan 162.85313 31 Bulgaria 31.60041

6
 1
1
2 United Kingdom 147.7496 32 Mexico 29.69187
1
3 Kazakhstan 141.45375 33 Philippines 28.45556
1
4 Ukraine 140.17408 34 Pakistan 25.34512
1
5 Canada 128.43991 35 Belgium 19.69026
1
6 Turkey 115.21266 36 Denmark 17.49116
1
7 Korea, North 67.59087 37 Chile 17.16074
1
8 Italy 62.57542 38 Slovakia 15.19382
1
9 Thailand 61.31154 39 Finland 14.76601
2
0 Czech Republic 57.58739 40 Bosnia and Herzegovina 14.29348
World 12897.92507

The Kyoto Protocol has long fulfilled its part as a policy governing the regulation of
greenhouse gases in an international scale. Among the mechanisms involved was the Clean
Development Mechanism wherein countries are highly encouraged to implement projects that
will help reduce the emission of greenhouse gases (United Nations Framework Convention on
Climate Change). This includes the application of scientific research, breaking ground for
innovations that could introduce solutions that are not only effective but also economically
friendly.

In the long run, there emerged several green innovations that were proven to reduce
global warming. However, reluctance in releasing these products due to economical and political
causes (Sy, 2008) only nullified the efforts made by the UN to achieve the said objective. In
other words, most companies find it difficult to give up the cheapest means of producing energy
and resort to it, even if it will contribute to global warming. As mentioned in Kirchsteiger’s
(2008) paper, the G8, otherwise known as the group of big eight countries have been supporting
the improvement of coal fired power-stations in its efficiency through the help of modern
technology, hence resorting to “capturing carbon dioxide”

2.1.3 Coal Consumption and CO2 Emission in the Philippines

Based on the latest updated statistics on coal consumption presented by Table 2.1 and
Table 2.2, Philippines ranked 34th in global coal consumption and 33rd in CO2 emissions
respectively. According to the DOE of the Philippines, industries that cater cement, energy
generators and other processes are the major coal consumers. Their recent studies (as of
December 12, 2006) show that out of the 9.5 million metric tons of coal, 73% is used for the

7
generation of energy, 22.5% is used for the processing of cement while the rest of the 3.75% is
used by other industries.

Considering this fact, Philippines is among the countries that consume considerable
amounts of coal without being able to implement effective methods that could either way reduce
or eliminate greenhouse gases.

2.1.4 Coal in the Philippines

According to the Department of Energy (DOE) of the Philippines, our country’s reserves
are scattered all over the Philippines, but the largest deposit is located in Semirara Island,
Antique, thereby also having the largest coal producer is Semirara Mining Corporation (SMC),
which contributes about 92% of the local coal production, but there are also coal mines located
in Cebu, Zamboanga Sibuguey, Albay, Surigao and in the Negros Provinces. According to the
DOE, and basing it on the 2006 Update of the Philippine Energy Plan (PEP), coal production in
2004 surpassed the 2003 level by 34% from 2.0 MMMT in 2003 to 2.7 MMMT in 2004, owing
to improved coal production of big mining companies as well as good weather conditions. Coal
production in 2006 as of December 12 stands 2.3 MMT run-of-min, 2.5% which came from
small-scale coal mining operations. The DOE claims that there are Philippines coals which are of
such high quality that they can be used without the need for coal preparation or blending with
imported coals, like the coal deposits from Malangas by the Philippine National Oil Company
(PNOC) with its Taiwanese partner, in Southern Cebu by Ibalong Resources and Development
Corporation (IRDC), and in Batan Island by Rock Energy International Corporation (REIC).

The coal to be used in this research is that mined by Semirara (Semirara Mining
Corporation). Semirara coal is classified as sub-bituminous. A pound of this fuel harnesses
energy that amounts to around 8600 Btu to 10450 Btu. Other contents that comprise the coal
exist in the following ratio: 11-15% moisture, 5-10% ash, 0.3-0.9% sulphur. The industrial grade
of Semirara coal particularly contains the following components as shown in table 2.3.

Table 2.3 Industrial grade Semirara coal constituents

obtained from the Semirara Mining Corporation

Gross calorific value, Btu/lb (air dried) 8650-9600

Proximate anlaysis (air dried, ASTMD3172)  
Ash, % 9-18
Fixed carbon, % 32-41
Volatile combustible matter 34-41
Total sulfur, % (air dried,
ASTMD2015) 0.40-0.90
Total Moisture, % (as received) 20-28
Residual moisture, (air dried), % 11-15
Hardgrove grindability index,% 40-50
Ash fusion temperature, ˚C  
Initial deformation temperature, 1120-1300

8
 ˚C
Hemispherical temperature, ˚C 1140-1380
Flow temperature, ˚C 1170-1490
Elemental ash analysis, % (dry basis)  
Sodium (Na2O) 2.00-4.00
Potassium (K2O) 1.00-2.00

2.1.5 Regulations implemented on Reducing CO2 Emissions in the Philippines

Laws and/or acts have been passed in the Philippines concerning the control of carbon
dioxide emissions and of other gases (greenhouse gases) imposing harm to Filipinos and to the
country’s physical nature. They have been formulated to directly serve the Philippines’
environment (air, land, water resources), to prevent damage and destruction of natural resources
and maintain clean, green and healthy surroundings.

Section 2 of the Climate Change Act of 2009 or Republic Act No. 9729 affirms that it is
the duty of the state to create policies protecting the people and providing them a clean and
healthy environment. The Philippine Agenda 21 allows for the fulfillment of this duty and
maintenance of a well and orderly environment. Furthermore, RA 9729 has been established to
protect the climate system and for its risk management. One of the primary objectives of this act
is to stabilize greenhouse gases to prevent the harm they cause – ecologically, socially and
economically. In line with this, projects and plans on climate change-related disasters must be
implemented. This policy is also in line with the global community’s policy towards climate
change. It is also stated in the policy that participation of other industries and institutions in the
realization of this act is a must. It is important to control climate change because as the section
two of this RA recognizes, the Philippines is susceptible to the consequences brought by climate
change (Klima Climate Change Center).

The Biofuels Act of 2006 or Republic Act No. 9367 is an act concerning Biofuel usage in
the country. The policy is in charge of lessening reliance on non-domestic fuels regarding the
country’s environment and human protection and economic growth. It also focuses on
improvement of livelihood with biofuels such as development of indigenous sources of
renewable energy, making clean alternative sources of energy (apart from imported oil) abundant
and available to all, alleviate greenhouse gases emissions, and increase in levels of income and
employment. The act encourages use of biofuels as a better alternative than gasoline and because
of its healthy benefits for the whole state (Senate of the Philippines).

The Philippine Clean Air Act of 1999 or Republic Act No. 8749 is an act concerning the
control of air pollution. Its principles are resting on the provision of clean air, harmonious
environment, healthy ecology and the human right to a clean surrounding and nature. It also is
the preventive measure for pollution but at the same time recognizes measures which are going
to help achieve the objectives of the policy. Section 3 of RA 8749 must pursue frameworks for
sustaining balance, development and protection of the environment. This section also writes that
there must be national and comprehensive programs for air pollution management; programs
which encourage cooperation and participation of the citizenry and industries in the management

9
of air pollution and which teach proper public information on air quality and on the ways to
maintain cleanliness and prevent air pollution (Environmental Management Bureau).

There are many laws that capture caring for the environment and provide support
for projects which have potentials in helping the government to achieve their goals. Many
environmental laws are leaning on the deterrence and/or treatment of toxic elements found in our
surroundings – gases.

2.2 Carbon Capture Technologies

Due to the impending degradation that coal consumption brought about, the search for
clean coal technologies began. Among the clean coal technologies discovered, carbon dioxide
sequestration is proved to be most suitable to allow the continuation of the demand and usage of
coal. As mentioned earlier, innovations resulted to numerous carbon capture technologies that
have various affects depending on the properties of gas and parameters applied on the capturing
medium. In this proposal, carbon capture technologies that are inclined to the incorporation of
thermodynamic chemical reactions, principles and processes are the scope of discussion. Among
the technologies known, chemical looping combustion and reforming (CLC/CLR), adsorption
and absorption are given focus in order to gain prior knowledge about the proceeding studies.

2.2.1 Chemical Looping Combustion or Chemical Looping Reforming

Chemical looping combustion (CLC) and reforming (CLR) are novel fuel conversion
technologies allowing inherent CO2 separation. Through the cyclic utilization of metal oxides to
bring oxygen to the fuel itself, the main advantage of this method is that there is no gas
separation step needed to get a concentrated CO 2 stream since air and gaseous products produced
after combustion of fuel were not mixed together (Yang, et al., 2008). Which means that energy
requirements are much lower that for pre- or post combustion capture or for oxyfuel combustion.
This technology was first introduced by Richter and Knoche (1983) and Ishida et al. (1987)
primarily to increase reversibility of combustion processes so as to utilize materials more
effectively. These systems consist of two reactors where different gas streams are in contact with
circulating solids, which transports oxygen and heat from one reactor to another. Metal oxides
allow such a transport. In the fuel reactor, fuel is oxidized by the metal oxide, and in the second,
which is called the air reactor, the metal oxide is reoxidized. If hydrocarbons are used as fuel in
CLC (although in princicple, any kind of major fuel can be utilized in CLC), the primary
products of the fuel reactor exhaust gas are CO2 and H2O. After condensation of water, a
relatively pure CO2 stream is left, which leaves a high potential for CO 2 capture, which is really
the main advantage of CLC because it avoids usage of too much energy. The air reactor exhaust
has consists mainly of nitrogen with some excess oxygen. In the study of Bolhàr-Nordenkampf
et al. (2009), two different Ni-based oxygen carriers in a 120kW chemical looping pilot rig was
used, and a dual circulating fluidized bed (DCFB) system was designed to obtain high solid
circulation, very low residence times and a high power solid inventory ratio, the pilot rig was
fuelled with methane at 140kW fuel power. For both oxygen carriers high CH 4 conversion and
CO2 yield is achieved. In this study, air to fuel ratio and temperature are varied. Higher air to fuel
ratio and temperature, decreased CH4 conversion, the problem with this is that they used the
word “seemed” to explain this phenomena connecting it to the Ni/NiO ratio, which very much

10
appeared like they didn’t find anything conclusive to really explain why this happened which is
why at their conclusion, they stated that further investigation is surely required (Bolhàr-
Nordenkampf, et al., 2009). Another study connected to this, is when they used natural ilmenite
and natural olivine (only as an additive) as an oxygen carrier material, this study showed that
there was reasonable conversion of CO and H2 but, the conversion of natural gas is relatively
low, but the adding of natural olivine resulted to a moderate increase of CH 4 conversion (Pröll et
al., 2009). This basically showed that natural minerals such as oxygen carriers aren’t as effective
as metals, when converting hydrocarbons. Another study by Jerndal et al. (2009), used 24
different oxygen carriers, based on NiO, with NiAl2O4 and/or MgAl2O4 and were produced with
spray-drying, and found that oxygen carriers supported by MgAl 2O4, or where a small amount of
MgO was added, displayed an increased fuel conversion when compared to oxygen carriers of
NiO supported by NiAl2O4, (Jerndal, et al., 2009) which is quite adverse, because, according to
most studies, Ni is the most effective oxygen carrier to convert hydrocarbons.

Another study, de Diego, presented results using CLR in a 900 ˚C circulating fluidized
bed reactor using a methane as fuel, again they used an oxygen carrier based on NiO and
supported on γ-Al2O3 was used during more than 50 hours of operation and the effect of
different operating variables like temperature, molar ratio and solid circulation rate on CH4
conversion and gas product distribution was analyzed. They found in all conditions, CH4
conversion was very high (greater than 98%) and the most important variable affecting the gas
product distribution was the solid circulation rate, that is NiO/CH4 molar ratio. During the
operation, it was found that the oxygen carrier particles maintained their physical and chemical
properties, which suggested the popular notion today that Nickel has a very high durability,
which makes it suitable to be an oxygen carrier for a CLR system which was actually used in the
aforementioned study (de Diego et al., 2008).

2.2.2 Adsorption

Adsorption is the process which will be used for this study. It is the process wherein a
substance of gas and liquid becomes attached to a solid; similar to absorption. The substance
adsorbed by the special solid is called an adsorbate. Adsorption happens every day in our
environment. The best examples of adsorbates are the pollutants in our environment such as
carbon and greenhouse gases (Mithra, 2010).

Many successful carbon capture experiments were done using the process of adsorption
and CO2 with a special solid. Plaza et al. (2007) affirmed successful CO2 capture depending on
the development of the special solid used and the adsorption capacity. In their study, they used
low cost sorbent. They sought different alkylamines as potential sources of sites for CO2 capture.
They also considered the effect of impregnation with the use of commercially activated carbon.
Their results showed that the amine coating, making the carbon more basic and also increased
the amount of nitrogen found in carbon, caused the significant decrease in microporous volume
of carbon. As a succeeding result, CO2 physisorption occurred, reducing raw carbon capacity.
Another study by Martín et al. (2010) showed the effectiveness of adsorption to capture carbon
through techniques on characterization of carbon. They used physical adsorption to determine
maximum capacity of carbon to CO2 before and after combustion processes. The adsorption
isotherms yielded the values of micropore volume and the energy characteristic of the carbons.

11
They followed on the theoretical framework of Dubinin’s theory. The analysis of these results
also gave the equilibrium CO2 uptake of the carbons at various temperatures and pressure. They
also noted special cases which resulted to higher values which indicated that CO2 uptake upper-
bound around10–11 wt% seemed more realistic for standard activated carbon after combustion.
The limit of the before combustion cases would not exceed 60-70%.

In the study of Plaza et al. (2010), they used almond shells as adsorbents for carbon
dioxide. They used the process of carbonisation followed by CO2 activation or heat treatment
with ammonia (amination). The said procedures resulted to CO2 with high adsorption capacity in
pure CO2 and in 15% CO2 in N2. Carbon dioxide activation produced porosity in most of the
micropore domain. Heat treatment with ammonia at 800 ˚C on the other hand, produced narrow
microporosity in the char and incorporated stable nitrogen functionalities enhancing CO2
selectivity. This process also gave greater carbon yield and shorter soaking time than CO2
activation (M. G. Plaza, et al., 2010).

2.2.3 Absorption

Absorption is another carbon capture process that involves the use of sorbent liquid
solvents, usually amine based solvents, to trap CO 2 gases, therefore separating it from the other
gases that would provide the heat required prior to energy conversion (Feron & Hendriks, 2005).
This can be applied in both combustion and pre-combustion stages but according to Feron and
Hendriks (2005), this process is favoured when decarbonisation was done at pre-combustion.
However, the hydrogen gas (H2) must be taken into account since this gas provides significant
amount of heat to power steam turbines or fuel cells.

First to be discussed are the parameters considered for different combustion stages where
absorption is to be employed. Absorption can be held at the pre-combustion stage or the post-
combustion stage. As said earlier, absorption decarbonisation is favoured at pre-combustion. In
order to avoid corrosion of equipment due to the acidic properties of CO 2 (Ma'mun, Svendsen,
Hoff, & Juliussen, 2007), absorption can be preferably done right after gasification of gases
before allowing entrance to the equipments. Furthermore, Pennline (2008) stressed the fact that
precombustion absorption requires gasification of fuel produces more concentration of CO 2
against CO, and then by design, collecting and transporting the CO2 through lower pressure at a
higher elevation, therefore making carbon capture process more effective. As for post-
combustion absorption process, the volume of the gas should be considered since carbon capture
requires the exiting gases to be at low pressure, and thus the design of high volume reactors (Alix
et al.). To address that problem, physical designs are incorporated along with absorption like
packed columns (Khan, Krishnamoorthi, & Mahmud) and specifically designed fabric
membranes of which their efficiencies conform to the principles of hydrodynamics (Alix, et al.).

Next is the selection of the solvent for absorption. According to by Aronu et al. (2009),
absorption efficiency of solvents would depend on physical properties such as its solubility,
vapour pressure, molecular mass, foaming tendencies and its ability to wear equipment, and also
including principles in physical chemistry such as reaction kinetics, energy regeneration and
cyclic capacity are also significant in analyzing the absorption capacity of solvent. In addition to
that, mass transfer of incoming gases and equilibrium between absorbed particles and absorbent

12
must also be considered (Blauwhoff, Versteeg, & Van Swaaij, 1983). Alkanoamines, like
monoethanol for instance, have been one most commonly used since industries sought to address
problems on pipe corrosion due to acidification of H2S and CO2. Its rate of reaction (being found
with utmost accuracy among all other alkanolamines) was given by the following as compiled
and formulated by Blauwhoff et al. (1983):

2152 1
log 10 k 2=10.99− (
T mol ∙ sec )
The availability of such data therefore makes monoethanolamine a good specimen to study
absorption. But for the other alkanolamines, equations cannot be justified due to the variations of
methodology and concentrations, as Blauwhoff pointed.

The use of MEA however is not economically friendly as it used to be. In fact, according
to Yang (2008), equipments that will have to control the parameters such like letting CO 2 react
with MEA to form a carbamate and heating it later for the release of CO 2. What Yang would like
to point out, basing upon the study conducted by Idem et al. (2005), was that the repetitive
regeneration and reheating of MEA actually constitutes 70% of an energy plant’s total cost.
Moreover, Yang also justified that MEA has a small CO 2 loading, it is easily worn out by other
absorbable waste gases such as SO2, NO2, HCl, HF and oxygen and it also corrodes
equipments(Yeh, Resnik, Rygle, & Pennline, 2005).

Recent studies proved that there are other solvents that could compete with the absorption
capacities of MEA in terms of cost and efficiency. One such study conducted by Ma’mun et al.
(2007) operated the screening apparatus illustrated in Figure 2.1 at 80˚C atmostpheric pressure to
observe the absorption/desorption capacities of the nearly pure assays following solvents:
monoethanolamine (MEA), 2-(butylamino)ethanol (BEA), N-methyldiethanolamine (MDEA), 2-
(methylamino)ethanol (MMEA), 2-(ethylamino)ethanol (EMEA), 2-(2-aminoethyl-
amino)ethanol (AEEA). In so far, AEEA exhibited an almost consistent, linear relationship of
loading CO2 and its capacity to absorb CO 2 from the water bath at 40˚C up until it reaches 80˚C
at the end of the cycle. Also, the fact that AEEA has a lower vapour pressure which indicates that
it has lesser volatility.

Figure 2.1 Rapid screening apparatus incorporated

in the methodologies of Aronu et al. and Ma’mun et al.
as obtained from Aronu et al. (2009)

13
 Another study conducted by Aronu et al. (2009), evaluates solvents of almost pure
concentrations (ranging from 85-99.9% by mass) namely monoethanolamine (MEA),
tetraethylenepentamine (TEPA), piperazine (PZ), 2-amino-2-methyl-1-propanol (AMP), N, N’-
di- (2 hydroxyethyl) piperazine (DIHEP), N-2-hydroxyethylpiperzine (HEP) and potassium salt
of sarcosine (KSAR). In this study, comparison of the efficiency of each sorbent was based off
monoethanolamine as a common material used in industrial operations. To determine the
sorbents’ the same screening apparatus for analyzing the solvents shown in Figure 2.1 was
utilized at the same conditions as the previous. Among the solvents TEPA was able to absorb the
most CO2 among other sorbents. However, there appeared to have a decrease in performance due
to viscosity when concentration is increased. Nevertheless, TEPA exhibits the capture of more
CO2 compared to MEA whose efficiency lowers upon continuous cycles. But since TEPA had
the least tendency of desorption, storing captured CO 2 and regeneration of this medium may be a
problem.

Although there may still be considerations in analysis, like for instance, taking into
account the differential increase in temperature as the gas travels through the apparatus, the lean
loadings (by mols of CO2 per mol of solvent) given the same reaction rate is sufficient to prove
that there are more economic alternatives than the use of MEA. It may still be necessary to
conduct experiments that could determine the diverse effects due to the different concentrations
on one particular solvent.

Besides the use of alkanolamine other amine derivatives, there also proposed the use of
ammonia (Resnik, 2004; Yeh, et al., 2005) as solvent and liquid sorbent-membrane systems that
uses chemical and physical means to sequester CO2 (Teramoto, Takeuchi, Maki, & Matsuyama,
2001). Since the main focus of the research is the ammonium absorption technology, this will be
discussed in detail in the following section.

2.3 Incorporation of Ammonia in Decarbonisation Absorption

Ammonia decarbonisation technology has not yet been employed in actual industrial
settings however Puxty et al. (2010) stated that ammonia has been proposed as a medium for
carbon capture due to its high loading, low energy requirement for regeneration and its resistance
against oxidation, although it has to be kept at a low temperature due to its volatility. Example of
procedures testing the loading of ammonia as compare to the commercial absorbent, MEA, is
based upon the mass of CO2 transferred upon passing through an absorbent wetted wall column
(Puxty, et al., 2010). The overall schematic diagram of the procedures used by the author is as
shown in figure 2.2. In the said procedures, temperature is kept low, ranging from 5˚C to 20˚C at
CO2 partial pressure range of 0 to 20 kPa which is different from the usual method of analyzing
the loading capacities of alkanolamines which are held at temperatures from 40˚C to 80˚C.
Results showed relationship of absorption flux as a function of CO 2 loading, temperature and
CO2 partial pressure of both solvents and comparison of the values. The end concluded that in
order for MEA can absorb CO2 around 1.5 to 2 times than ammonia does. However, MEA will
have to be kept at a temperature not lower than 40˚C, whereas ammonia could be used at
temperatures as ambient as 20˚C. But in order to make up for the decrease in reactivity with the
lowering of temperature, a larger contact area by enlarging the dimensions of the absorber
column.

14
 Figure 2.2 Schematic diagram of the procedures used by Puxty et al. (2010)
in determining the load capacities of ammonia and MEA

In addition to the problems that may yet be encountered in using ammonia to replace
alkanolamines would be the energy requirement for the compressor for refrigeration and the
fouling of the stripper at temperatures below 50˚F(Mathias, Reddy, & O'Connell, 2009). Mathias
et al. (2009) pointed that an increase in pressure is one way to physically reduce the energy
needed for compression.

For the regeneration of ammonia, Yeh et al. (2005) showed and stressed that the reaction
mechanisms involved during the dissociation of ammonium bicarbonates to CO 2 and H2O have
the lowest enthalpy. In addition to that, the exhibited release of CO2 as shown in the said author’s
results accounts to 60% to that of the total CO 2 originally absorbed. There also stated a
precaution procedure in handling absorbed gases, where cold water (at 4˚C) is mixed with the
laden absorbent to avoid the evolution of gases before sealing. Having defined other factors to be
taken in account for the study of ammonia absorption, Yeh and his colleagues’ paper may serve a
good introduction. Details about the theoretical perspectives obtained will be discussed in the
next chapter.

15
 Chapter 3: Theoretical Framework

3.1 Chemical Properties of Ammonia

Ammonia (NH3) is a weak alkaline inorganic compound (Qin, Wang, Hartono, Svendsen,
& Chen, 2010) consisting of one nitrogen atom bonded to three atoms of hydrogen. Two free
electrons on the nitrogen atom allow this compound to attain a trigonal pyramidal structure.

The physical properties of ammonia recorded in Perry’s Chemical Engineering Handbook

(Green & Perry, 2008) are summarized in table 3.1. There, it can be seen that ammonia attains a
specific gravity of 0.817 at -79˚C while the specific gravity if 0.5971 at ambient temperature.
Boiling point is at -33.4˚C at atmospheric pressure which therefore classifies ammonia as a
highly volatile compound. To retain its liquid form, ammonia will have to be mixed with
solvents with lesser volatility while vapour pressure contributes to the compression of molecules
into liquid form as did Rivera-Tinoco et al. (2010).

Table 3.1 Physical properties of ammonia (NH3)

obtained from Perry’s Chemical Engineering Handbook

formula weight 17.03

refractive index 1.325 (lq.)
specific gravity 0.817−79°
  0.5971 (A)
melting point (˚C) −77.7
boiling point (˚C) −33.4
solubility in 100
parts:
cold water 89.90°
hot water 7.496°
other solvents 14.820°

Since low pressure drops are expected upon the entry of the CO 2 gas into the reactor,
vapour pressures much lower than 1atm must be achieve. Furthermore, since ammonia is less
likely to saturate given the operating temperature (20˚C) which is still near ambient, maintaining
ammonia in its liquid form will once again depend on the partial pressure the incoming flue gas
exerts. The following vapour pressures of 1 mmHg to 760 mmHg and their corresponding
temperatures are summarized in table 3.2 as obtained from the previous source.

Table 3.2 Vapor pressure of ammonia (NH3) and corresponding temperature

as obtained from Perry’s Chemical Engineering Handbook

Pressure, mmHg Temperature, °C

1 −109.1

16
 5 −97.5
10 −91.9
20 −85.8
40 −79.2
60 −74.3
100 −68.4
200 −57.0
400 −45.4
760 −33.6

3.2 Reactions Involved in Ammonia Decarbonization

Several journals have stated the reaction mechanisms involved in vapour-liquid

equilibrium in literature. Darde et al. (2009) listed down the equilibrium reactions that were
observed in a CO2 –H2O-NH3 during the absorption process. Among the reactions were the
following as shown in table 3.1:

Table 3.3 List of equilibrium reactions involved

in ammonia absorption

Speciation equilibria
−¿ ¿ + ¿¿

N H 4 ( aq ) + H 2 O↔ NH +¿+OH ¿
CO 2 ( aq )+ H 2 O ( l ) ↔ HCO−¿+H ¿
4 (1) 3 (2)
+¿ ¿
2−¿+ H ¿ + ¿¿
−¿ ↔CO −¿+H ¿
HCO3 3 ¿
(3) H 2 O ( l ) ↔ OH (4)
−¿+ H 2 O ¿
NH COO
NH 3 ( aq ) + HCO−¿↔ ¿
3
2
(5)

Vapor-liquid equilibria
CO 2( g) ↔CO 2 (aq) (6) NH 3 (g) ↔ NH 3 (aq) (7)
H 2 O(g) ↔ H 2 O(l) (8)

Liquid-solid equilibria
−¿↔ NH4 HCO3 ( s) ¿ 4
−¿↔ NH2 COON H (s )¿
HCO NH COO
NH +¿+ ¿
NH +¿+ ¿
4
3
(9) 4
2
(10)
(11) H 2 O(l)↔ H 2 O(s)
2−¿+ H 2 O ↔ ( NH 4 )2 CO3 ∙H 2 O( s) ¿

2 NH +¿+CO 3 ¿
(12)
4
−¿ ↔ ¿
2−¿+ 2 HCO 3 ¿
+¿+CO 3 ¿
4 NH 4
( NH 4 )2 CO3 ∙ 2 NH 4 HCO3 (s ) (13)

The author noted that among those equilibrium reactions, five of them include the
formation of solids namely ammonia bicarbonate (NH4HCO3), ammonia carbonate
((NH4)2CO3·H2O), ammonia carbamate (NH2COONH4), sesqui-carbonate
((NH4)2CO3·2NH4HCO3) and frozen water. The capability of forming these solids is something
to be considered when designing since as Yeh(2005) says, this could build up on walls and
eventually clogging pipes at prolonged accumulation.

17
 Aside from the formation of solid crystals, reactions under the liquid-solid equilibria
show that the left side is consisted of binary to ternary reactants of heterogenous gas liquid
mixtures. There, it can be seen that Le Chatelier’s principle may apply, in which states that
application of pressure at the side containing more reactants may shift the reaction into forming a
more compressed product (Maron & Lando, 1974). Hence, pressure plays a significant role
optimizing the absorption of CO2 with ammonia.

3.3 NH3-CO2 –H2O Equilibrium Diagram

Since aqueous NH3 form crystals with CO2, factors such that the composition of three
compounds must be considered in order to facilitate the flow of gases while controlling the
amount of crystals while in contact. To give a fundamental introduction of the appearance of the
three liquid diagram, figure 3.1 is as presented by Thomsen’s Extended UNIQUAC model in
comparison to Jänecke’s (1917) findings.

Figure 3.1 Ternary diagram of NH3-CO2 –H2O system at 40˚C and 1 bar
as presented in UNIQUAC model

The solid-liquid ternary diagram is a Type II: Binary Compound Formation in terms of
Maron and Lando’s (1974) classification. The blue lines represent tie lines of which systems
compositions enable the precipitation of solids indicated while the black line is that solely for the
formation of hydrated ammonium carbonate. However, this may not be a reliable basis for
determining the equilibrium systems at 20˚C which has yet to be analyzed.

3.4 Absorption

Absorption is defined as the introduction of inert gas into solvent wherein which the
former will be soluble (McCabe, Smith, & Harriot, 2005). McCabe (McCabe, et al., 2005)
mentioned that the principle of absorption has been used in obtaining high concentrations of gas
solute and the remaining solvent maybe discarded and reused. The author further added that the
opposite of such operation is known as stripping or desorption wherein there involved the
counter flow of an inert gas upon contact with solute laden absorbent.

18
 Since the thesis only covers the absorption capacities of different ammonia
concentrations, the focus will be on mass transfer and physiochemical properties.

3.4.1 Material balance

For any reactor used in absorption, the material balance is as follows:

La x a+V b y b =Lb x b +V a y a (McCabe, et al., 2005)

where L and V represent the molal flow rates, x and y represent the mol ratios of solute in liquid
and gas phase respectively. Subscripts a and b indicate the input and output positions
respectively.

3.4.2 Limiting Gas-Liquid Ratio

When operating the absorption column, it is important to know the limiting gas-liquid
ratio (L/V) to ensure that the process is done efficiently and economically. Based on findings by
Qiu et al. (2010), the overall volumetric mass transfer coefficient with respect to gas-liquid ratio
is as follows:

Figure 3.2 Overall volumetric mass transfer coefficient vs.

gas-liquid ratio (Qiu, et al., 2010)

It can be seen clearly that the increase in overall volumetric mass transfer was due to the increase
in solvent which is the 10% (v/v) aqueous ammonia. With the liquid-gas ratio at 0.0089, the
overall volumetric mass flow reaches its highest (Qiu, et al., 2010). However, the line seems to
deflect horizontally as it goes beyond which indicates that further increase in solvent’s molal
volumetric rate will not result into any significant increase in absorption efficiency. Therefore in
this research, gas-liquid ration to be observed will be at 0.007 for all concentrations.

3.4.3 Multicomponent Absorption

Since combustion of fuels such as coal are not often complete, there will be components
such as CO2, CO, O2, H2, N2 and SO2. Although it is not yet certain which of the gases except
nitrogen shall be absorbed, the material balance for multicomponent absorption is given by:

19
 V ( y B , b− y B ,a ) =L(x ¿B , b−x B ,a ) (McCabe, et al., 2005)

where subscript B represents component B of the system, a and b represent the input and output
positions respectively. yB and yA is the mol fraction of component B in vapour phase and liquid
phase respectively. xB* is the mol fraction of solute in equilibrium with the liquid phase.

3.5 Wetted-Wall Column

Simple laboratory settings for the determination of CO 2 of absorption of different

solvents involve the use of wetted-wall columns (WWC) as reactors (Liu, Wang, Zhao, Tong, &
Chen, 2009; Puxty, et al., 2010). Wetted-wall columns simulate packed tower reactors such that
both involve the counter flow of two different fluids (Puxty, et al., 2010). However the
difference is the liquid inlet that is made to flow through a smaller cylinder which is the column,
bound by an outer metal jacket. Liu et al. (2009) this instrument is first used by Mshewa (1995),
and was since then commonly used by other researches involving the test of absorption.

One of the most recent studies conducted by Qian (2009), using the modified wetted-
wall column made of 1mm spaced steel tube annulus column and 23mm spaced annular jacket
(where water bath circulates) exhibits the liquid film thickness of N-methyldiethanolamine given
by this equation:
1
Q 2 2

ĺ d , mod =(L/t c
+π R

π )−R

Where Q is the volumetric flow rate of the solvent, L is the length of the column, t c is the contact
time and R is the radius of the inner of the column annulus. This equation may prove crucial in
determining the limiting factors when operating the column since increase in thickness (as
related to the mass) of the solvent may dilute the solute gas which is to be avoided since it makes
stripping of CO2 gas difficult (McCabe, et al., 2005). However, that is only to approximate the
workable design since that equation is applicable when no CO 2 is yet loaded and when operation
is done at atmospheric pressure (Qian & Guo, 2009). Hence, say the wetted-wall column used by
Puxty et al. (dimensions for for height and diameter are 0.0821m and 0.0127m respectively) will
be converted to one such like Qian’s, while maintaining film thickness of 1.15×10 -4, the
volumetric flow rate should be at 0.38 mL/s. Calculation is shown in the appendix A.1.

20
 Chapter 4: Materials and Methodology

4.1 Materials

Carbon dioxide source to be used in this thesis will be from the flue gas produced from
the combustion of Semirara industrial grade coal. Absorption of flue gas from the combustion of
10g sample of coal shall be tested upon 10 g samples of aqueous ammonia solutions of different
concentrations: 0.1M, 0.2M, 0.3M, 0.4M, 0.5M and 0.6M. Reactor model shall be based upon
Qian’s (2009) model where dimensions applied will be the same as that of Puxty’s (2010)
wetted-wall column. The following dimensions are as follows: annular metal column with 1mm
space and inner diameter of 1.27 cm and outer diameter of 1.37 cm for the plastic tube (assuming
metal sheets). The height of the column remains stationary at 8.21 cm. Annular Pyrex glass
jacket with an internal diameter of 2.54 cm and an outer diameter of 5.04 cm including inlet and
outlet for the water bath. Aperture for the gas inlet however will be enlarged to 10mm for a
greater pressure drop at the end of combustion. Steel flanges that seal the reactor will have
indentions where thermometer can be placed for the monitoring of temperature. Also, another
glass enclosure is provided to protect the mechanism and allow the monitoring of process. In
order to show the basis of design, figure 3.2 is provided. Specific materials used as described
below the figure may not necessarily apply in actual fabrication for this procedure.

Figure 4.1 Qian’s wetted-wall column design

Lastly, it will require gas analyzing instruments such as gas spectrometers to analyze the
content of gases, before and after the absorption is to be done.

4.2 Experimental Setup

For quick reference, the diagram setup is illustrated in figure 4.2.

Figure 4.2 Experimental setup

21
 Air

Semirara
Temporary

source
Coal

Heat
Storage

Circulating Water Bath

Gas
Gas
Condenser Spectrophoto
Conditioner
meter
Pressure
Regulator
with Flow
Meter
Saturator Wetted-
Wall
Water Bath Column

Sample
Reservoir Cold
Water

This is derived from Puxty’s et al. (2010) experimental setup however there are a few
modifications since combusted coal fuel gas is used. At the heat source, Semirara coal is
combusted with theoretical air. Since a large amount of heat is expected to evolve, flue has is
stored temporarily in flask submerged in circulating water bath. Once cooled, gas will be
introduced to the saturator (1/8” stainless steel coil) maintaining a CO2 partial pressure of 20
kPa. Meanwhile, 10 grams of aqueous ammonia sample will be placed in water bath while being
circulated with a volumetric rate of 0.83 mL/s through the annular space of the wetted-wall
column by the use of pumping force. As for the outer annulus, cold water of 20˚C will be
circulated through the annular space of the outer glass jacket.

4.3 Experimental Procedures

The following procedures to be done in the experiment are presented in chronological

order.

4.3.1 Combustion of Semirara Coal

As mentioned in the earlier sections, before the absorption of aqueous ammonia will be
tested, the composition of the flue gas from combusted Semirara coal (10 gram sample) must be
determined separately from the experimental set up. To ensure the accuracy of data, five trials
will be held to obtain five records of the flue gas composition (CO 2, CO, H2, H2O, O2, N2, SO2).
Coal will be combusted such that only ashes remain and there added five minutes of heating after
the solid fuels are no longer visible. As for the theoretical air to be introduced, computation will
be based upon the data provided by the Semirara Mining Corporation with the assumption that
fuel undergoes complete combustion. After the analysis with gas spectrophotometer, the average
of five records for each gas composition will be computed for and used for theoretical
calculation in material balance.

For the actual determination of absorption, another 10 gram sample will be combusted in
the same manner as did the previous five trials. Flue gas will be temporarily stored inside a flask
while being gradually cooled in a circulating water bath. Partial pressures of solute gas may be
calculated theoretically with gas correlations to determine the control pressure to attain desired
gas velocity.

22
4.3.2 Preparation of Aqueous Ammonia Sample

For the variation of solvent absorbents, ammonia shall be diluted in water in the
following molarities: 0.1M, 0.2M, 0.3M, 0.4M, 0.5M, and 0.6M. These will be loaded into the
sample reservoir and pumped within the reactor. No carbon dioxide loading will be done
beforehand.

While flue gases are left to cool, 10 g of aqueous ammonia sample will be first placed in
water bath for five minutes until it comes to thermal equilibrium. Then liquid will be made to run
0.38mL/sec and will be indicated by an orifice meter.

4.3.3 Absorption Determination

While flow rate of solvent is maintained constant and the molarity increases, there should
be an equivalent decrease in flow rate for the incoming flue gas. Gas flow rates for each
corresponding molarities above will depend on the partial pressure of CO 2 of the flue gas to be
analyzed. The gas flow rate will be controlled with the pressure regulator.

Cooled flue gas will be made to pass through the saturator, then to the column counter-
currently with the solvent sample to be tested. Unabsorbed flue gas composition will then pass
through the condenser, conditioner and then be analyzed with the gas spectrometer until liquid
and gas finally comes into equilibrium. Then the unabsorbed flue gas after the equilibrium will
be recorded. For the next five molarities, another 10 g sample of coal will be loaded, combusted
and cooled, and 10 g sample of solvent to be placed in the water bath to attain thermal
equilibrium in preparation for another analysis.

Figure 4.3 Flowchart of procedures

Five trial determination of composition of flue

gas from 10 g samples of Semirara Coal

Determination of average composition from 5

trials and partial pressure of CO2 for the
attainment of desired flow rate

Preparation 10 gram samples of aqueous

ammonia with the following molarities: 0.1M,
0.2M, 0.3M, 0.4M, 0.5M, and 0.6M.

Combustion of new 10 g coal sample and

Recording of unabsorbed flue gas after
temporary storage of flue gas inside a flask
equilibrium.
while cooled in a circulating water bath

Attainment of thermal equilibrium of currently

Saturation and introduction of cooled flue gas
tested ammonia sample in reservoir placed in
into wetted-wall column.
water bath

Pumping of aqueous ammonia sample at .38

mL per seconds as indicated by an orifice
meter.

23
 References

Alix, Pascal, Raynal, Ludovic, Abbe, François, Meyer, Michel, Prevost, Michel, & Rouzineau,
David. Mass transfer and hydrodynamic characteristics of new carbon carbon packing:
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Allied Deviation. Material Safety Data Sheet: Ammonia Retrieved 27 November, 2010, from
http://www.alliedaviation.com/locations/pipeline/MSDS.pdf

Aronu, Ugochukwu E., Svendsen, Hallvard F., Hoff, Karl Anders, & Juliussen, Olav. (2009).
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DOI: 10.1016/j.egypro.2009.01.139

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Bolhàr-Nordenkampf, Johannes, Pröll, Tobias, Kolbitsch, Philipp, & Hofbauer, Hermann.

(2009). Performance of a NiO-based oxygen carrier for chemical looping combustion and
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10.1016/j.egypro.2009.01.005

Darde, Victor, Thomsen, Kaj, van Well, Willy J. M., & Stenby, Erling H. (2009). Chilled
ammonia process for CO2 capture. Energy Procedia, 1(1), 1035-1042. doi: DOI:
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28
 Appendix

A. Calculations

A.1 Approximation of flow rate of aqueous ammonia

through the equation suggested by Qin (2010)
2
π ( ( ĺ d ,mod + R ) −π R2 ) L
Q=¿
tc

0.0127 2 2
0.0127

Q=
[( −4
π 1.15 ×10 +
2 ) (
−π
2 ) ] 0.0821
1

−7 m3 cm3
Q=3.8 × 10 ∨0.38
s s

29
B. Materials Safety Data Sheet

B.1 Ammonia

Description
Chemical name: Anhydrous Ammonia CAS registry number: 7664-417
Synonyms: Ammonia Formula: NH3
Chemical family: Inorganic Molecular weight: 17.03
Composition: 99~% Ammonia  
Physical Properties Hazard Description
Boiling point -33°C (-28°F) Not recognize by OSHA as a carcinogen.
Freezing point -78ºC (-108°F) Not listed in the National Toxicology Program annual report.
Not listed as a carcinogen by the International Agency for
Flash point none
Research on Cancer.
651 ºC (1204ºF) catalyzed
Conditions to Avoid
Self-ignition by iron
temperature 850 ºC (1562ºF) Mixing ammonia with halogens, strong oxidizers, strong
uncatalyzed mineral acids, Nitric
Flammable limits in LEL 15% Acid, Fluorine, Nitrogen Oxide, etc…
air UEL 28% Explosive combustion result with mixture of air and the
Specific gravity following: hydrocarbons, Ethanol and Silver Nitrate, Chlorine,
0.682 @ 4°C (39°F) etc….
(water=1)
Vapor/air (air=1) 0.596 @ 0°C (32°F) Reaction with Silver Chloride, Silver Oxide, Bromine, Iodine,
Gold, Mercury,
Vapor pressure 10 atm @ 25.7ºC Tellurium Halides, etc. form explosive products.
89.9 g/100cc @ 0ºC Ammonia may form hazardous reactions with the following:
Solubility in water Silver, Acetaldehyde, Acrolein, Boron, Halogens, Perchlorate,
7.4 g/100cc @100ºC
Chloric Acid, Chloric Monoxide, Chlorites, Nitrogen
Surface tension 23.4 Dynes/cm @ 11.1ºC Tetroxide, Tin, Sulfur, etc….
Percent volatile 100%
Ammonia can corrode galvanized surfaces, copper, brass,
Appearance and Colorless gas/liquid and bronze, aluminum alloys, mercury, gold, and silver.
odor pungent odor
Stable at room
Hazardous Decompositions
temperature
Reactivity
Will react exothermicall Hydrogen and nitrogen gases above 450ºC (842ºF) can form
with acids and water high heat. Reaction with metals may help dissipate heat
Exposure limits
Federal OSHA PEL 50 ppm 8 hour (TWA)
NIOSH REL / ACGIH TLV 25 ppm 10 hour (TWA)
  35 ppm 15 min. (STEL)
IDLH 300 ppm  

30
 Emergency Treatment
Hazard/Symptoms Preventive Measures Fire Extinguishing/First Aid

Lacrimation, edema Flush eyes with abundant amount of water

or blindness to the Wear goggles when handling chemical for 15 minutes with eyelids held away
eye. from each other, exposing the eyeball.

Irritation, corrosive Remove contaminated clothes and gears

burns, blister and flush inflamed skin with abundant
formation on skin. Wear personal protective equipments (PPE) amounts of water for 15 minutes. Carefully
Caustic burn may at all times until after the cleaning and remove contaminated attire in case of
result from tissues keeping of equipments. material frozen to skin that might cause
freezing upon further abrasions. Do not apply any salves
contact. or ointment.

Acute irritation of
respiratory tract,
bronchospasm, Wear masks. Peform transfer under the Move to area with fresh air. Apply oxygen
edema or respiratory hood where vapors are drawn away. or artificial respiration if unconscious.
arrest upon
inhalation.
Lung irritation,
pulmonary edema
and other symptoms Avoid eating, drinking or smoking inside Give plenty of water or citrus juice to drink
similarly occuring in the lab if conscious. Do not induce vomiting.
inahalation may
occur upon ingestion.
Formation of
explosive compounds
and/or reactions as Wear protective clothing and pressure
Properly label container. Keep away from
mentioned in postive SCBA. Cool fire exposed
heat and distance it from other chemicals.
Conditions to Avoind containers with water spray while upwind
and Hazardous
Decompositions

*There are no chronic effects.

*Spasms, inflammation or edemas due to extreme exposure may cause death.

Notes:
*To physician, lung injury and pulmonary edema may not appear immediately. Therefore
supportive treatment and ventilation should be provided to make sure.

*FOR ALL EXPOSURES, SEEK MEDICAL ATTENTION IMMEDIATELY.

31
 Spillage Waste Disposal Storage and Handling Labeling/NFPA
While wearing protective attire Ammonia may be used for Considering ammonia as a 3 - Health,
and respiratory protection, and manufacturing fertilizers hazardous material, it 1 - Flammability,
spray water downwind. Isolate but should be kept from should be kept in a cool, 0 - Reactivity,
diluted run-offs from sewers entering bodies of water. well-ventilated area with H- Personal
and bodies of water. Disposal should comply container sealed tightly. Protection
CAUTION: adding water with environmental
directly to liquid spills increase legislations.
volatility of ammonia, thus may
result to increase in exposure of
environment

*Information for materials safety data sheet is obtained from Allied Deviation

32
B.2 Lignite or Sub-bituminous Coal Fly Ash

Description
Product/Chemical name: Coal Fly Ash CAS registry number: 68131-74-8
Synonyms: Ashes(residues),coal ash, fly ash
Physical Properties Health hazards
Boiling point > 1000° C Exposure route: Inhalation
Freezing point none Skin Contact
Flash point none Eye Contact
Self-ignition
temperature none Ingestion
Crystalline Silica is classified by
Specific gravity 2.2-2.8 Note: IARC as human carcinogen.
Vapor density not measurable
Vapor pressure Not measurable Personal Protective Equipment
Respiratory
Solubility in water < 5% Protection: Appropriate mask
Light tan or beige
Solid powder Eye Protection: Goggles
Reactivity Reacts with water Skin protection: Gloves, shoes and
    protective clothing
Emergency Treatment
Hazard/Symptoms Preventive Measures First Aid
Inhalation Wear mask. Move person to fresh air.
Contact emergency medical support
if the person is not breathing.
 
Rinse thoroughly with water at an
Eye Contact Wear google in handling coals. eye station. Do not rub. Seek
medical attention as soon as
  possible.
Wear appropriate gloves Wash contaminated skin
Skin Contact immediately with water and soap.
and proper clothing.
Seek medical attention for skin
  irritation.
Ingestion Avoid eating in the working area. Do not induce vomiting, but drink
plenty of water.

33
 Waste Disposal Storage and Handling
Ammonia may be used for manufacturing fertilizers Avoid accidental release. Store dry and away from
but should be kept from entering bodies of water. water. Dispose of containers in an approved landfill or
Disposal should comply with environmental incinerator.
legislations.

*Information for materials safety data sheet is obtained from Lafarge North America (2002)

34