Chapter II

10
 CHAPTER-II
Instruments and Methods

2.1 Introduction
As mentioned earlier, the technology for conversion and utilization
of biomass residues in their mixed forms needs small appropriate
adoption in the existing devices using fossil fuels since their
characteristics related to combustion are different from those of fossil
fuels. While detailed analysis of characterization of variety of bio
residues in their natural form are now available (Grover P.D. et al, 1989)
characterization of their mixtures needs further studies and
systematization. The present work is a modest attempt in that direction
related to a few combinations of bio residues available around us. In this
chapter we try to discuss the instruments used in such characterization
along with the methods we used in preparing the mixtures of bio residues.

2.2 Collection of samples:

The bio residues needed for the present study were chosen based
on the availability and the abundance of them. In Tamil Nadu and
especially in and around Madurai rice husk and ground nut shell are very
much available. In addition to these two bio residues saw dust was chosen
as the next bio residue due to availability in abundance from the timber
and wood industries surrounding Madurai.

The rice husk was collected from the rice mills located near
Palanganatham. The saw dust was collected from the timber industries
near Thirumangalam. The ground nut shell was collected from the
decorticating units near Solavandhan.

11
 The materials collected were first cleaned by hand by removing the
unwanted materials such as stones, dry leaves etc. The samples were then
sieved using simple manual sieves to get particles of approximately the
same size (1000 to 2000microns) .The samples were then air dried for
two days and then packed in polythene sacks.

2.3 Preparation of samples:

Rice husk and saw dust as host materials were used as such to
prepare the sample of required fineness. But ground nut shell sample was
made into small sizes by using ordinary mixer initially. The samples thus
prepared were purged with N2 gas to drive out the entrapped air
containing O2 to avoid auto oxidation. Grinding the above three samples
to get the required size was done by using RETSCH Ultra centrifugal
Mill ZM200. In the Ultra centrifugal Mill the samples were fed through
the hopper into the grinding chamber. The sample size was reduced by
the action of the high speed rotor. When the required fineness was
reached the centrifugal force expelled the sample through the ring sieve
and the sample output of approximately 200 microns was collected in the
collecting pan. The samples thus prepared were kept in air tight polythene
covers. The photographs of the three host materials as in their native
form, in the powdered form and in the charred form are shown in Figure
2.1.

12
Figure 2.1 Rice husk, Saw dust and Ground nut shell in their native form,
powdered form and in their charred form

13
2.4 Instruments used:
The instruments used to carry out the required characterization
studies are detailed in this unit. The Instruments at department of Physics,
Thiagarajar College of Engineering, Madurai, Magneto Hydro Dynamics
division, Bharat Heavy Electricals Ltd, Trichy, Indian Institue of Science,
Bangalore are used for the characterization studies.

List of instruments used for characterization studies:

• Electronic Balance
• Muffle Furnace
• Ball Mill Unit
• CHN Analyzer/Elemental Analyzer
• Bomb Calorimeter
• Flammability Apparatus
• TGA-Thermo Gravimetric Analyzer
• SEM-Scanning Electron Microscope

The working principle, description and operating procedures of the above

mentioned instruments are given below.

2.4.1 Electronic Balance:

The electronic balance used for taking all measurements is Adair

Dutt 60 B balance, marketed by Adair, Dutt Instruments Pvt Ltd and
manufactured by Chyo, Ymc Co, Ltd, Japan.

This balance can hold maximum 60 g of the sample and the

readability is 0.001 g. The balance is placed in a controlled environment

14
and protected from air currents. The shield helps to avoid such drafts. The
ambient temperature & humidity are maintained. The balance is placed in
a table with leveled surface & the table must be free from excessive
vibrations.

The sample has to be placed at the center of the sample pan to

avoid slight errors. The balance has to be calibrated initially for the best
performance. The most accurate calibration is made only after the balance
has been connected to a power source for 30 minutes.

The calibration procedure is as follows: Check the spirit level of

the balance and adjust if necessary. Make certain the weighing pan is
empty. Press the F key until “Cal” appears in the display. Press the TARE
key within two seconds to start calibration. The balance automatically
sets zero. The balance will then request appropriate size calibration
weight. For the balance we are using (AD 60B) the calibration weight is
50g. Place 50g weight in the weighing pan and wait for 10 seconds. Then
press the TARE key. “Pass” appears in the display when the calibration is
successfully completed. Now the balance is ready for use and we can
make measurements with 0.001g sensitivity.

The photograph of this electronic balance and another electronic

balance used for measuring weights greater than 25g and less than 60g
are shown in Figure 2.2.

15
Figure 2.2 Electronic Balance

16
2.4.2 Muffle Furnace

The muffle furnace is used to do the proximate analysis of the

biomass fuels and also to prepare the charred form of the biomass fuels.
The muffle furnace available in the Department of Physics, Thiagarajar
College of Engineering is used for this study. This furnace has a digital
temperature controller. It helps to fix the temperature at the desired level.
The digital display reads the temperature fixed and the current
temperature. Temperature setting buttons are also available on the panel.
The maximum permitted temperature is 1000˚C. The furnace has a
sensitive Pt-Rh thermo couple to detect the temperature variation.
Filament heating technique is used to heat the chamber. The heating is
carried out in the atmospheric conditions. The heating chamber has a
dimension of 15cm × 15cm × 20cm. At a time up to 4 silicon crucibles of
15ml capacity can be placed inside the heating volume. The heating
volume is insulated from the surrounding with fiber bricks.

Most of the heating requirements for the presents study are met
with the muffle furnace. In addition to this an electrical furnace is also
used for few cases. This electrical furnace can be operated in air and
nitrogen atmosphere. The diagrams of the furnaces are shown in Figure
2.3.

17
 Full View

Heating Volume

Figure 2.3 Muffle Furnace

18
2.4.3 Ball Mill Unit

The Ball Mill Unit is capable of giving excellent grinding results

even with difficult sample materials. The Ball Mill Unit used for grinding
our bio residue samples is RETSCH’s Ultra Centrifugal Mill ZM 200.
This milling unit far exceeds the performance and speed of any other
rotor mill.

This unit has a speed range of 6000 to 18000 rpm and the
circumferential rotor speed is more than 300 Km/h. The high sample
through put power of the unit is achieved by a perfectly matched
frequency converter and three phase motor. One of the special features of
this milling unit is patented cassette system for 100% sample recovery.
One can use sample volumes from 10 to 4500ml in this machine with
fineness down to 40µm. Above all this RETSCH’s Ultra Centrifugal Mill
is very easy to operate and it is very safe to handle.

This Ball Mill Unit is used to grind our biomass samples. The three
host materials are first grind to approximately 200 microns size. The
samples thus prepared are then mixed in required proportions to carry out
the further study. The diagram of the Ball mill unit is shown in Figure 2.4.

19
Figure 2.4 Ultra Centrifugal Mill

20
2.4.4. Elemental Analyzer/CHN Analyzer

The Elemental Analyzer CE 440 is widely regarded as the

instrument that sets the standard for CHN analysis. The oxygen flask
combustion unit present in this analyzer is designed to be a safe method
for igniting samples. The combustion that takes place is a simple
procedure involving a few mm of absorbent solution in a flask. The
sample is placed in an ash less filter paper holder and weighed out. This
method is set up with minimal cost and can cope up with a wide range of
samples.

Since the potential explosions are contained within the unit it is

very safe to use this instrument. The combustion is carried out in a sealed
flask enabling minimum product leaks. There is one additional safety
measure that the combustion unit will not operate whilst the door is
opened. Altogether this elemental analyzer is very simple to operate and
excellent to get reliable results.

The elemental analyzer available at Organic Chemistry Laboratory

of Indian institute of Science, Bangalore is used for the present study.
Samples were given and then the reports were collected.

In our study to do the ultimate analysis and to know the

composition of the biomass samples in weight % of the major
components oxygen as well as sulfur and nitrogen are determined using
the elemental analyzer.

21
2.4.5 Bomb Calorimeter:

This instrument provides a simple and inexpensive method for

determination of heat of combustion of organic matter and the calorific
value of solid or liquid fuel.

With this digital bomb calorimeter calorific value of different

biomass samples can be measured as per recommendations of British
Standard Institutions (BS 1016 Part 5-1976) Standard Institutions (IS
1359-1959) Institute of petroleum (IP 12/63 T .Appendix)

The bomb calorimeter will measure the amount of heat generated

when matter is burnt in a sealed chamber (bomb) in an atmosphere of
pure oxygen gas. The Photograph of the Bomb Calorimeter is given as
Figure 2.5. The schematic diagram of the Bomb calorimeter is shown in
Figure 2.6. The block diagram to connect ignition wire cotton thread and
sample is given in Figure 2.7. The block diagram of oxygen filling in
Bomb with safety device is presented as Figure 2.8.

The sample placed in the bomb is ignited electrically. As the

sample burns, heat is produced. The rise in temperature is determined.
The water equivalent of the calorimeter assembly is also known by
equating the amount of heat produced by burning to the amount of heat
absorbed by the sample can be calculated

Let W=Water equivalent of the calorimeter assembly in cal/c

T=Rise in temperature in c

H=Heat of combustion of material in cal/gm

M=Mass of the sample burnt in gm

Then WT=HM Knowing W, T& M, and H can be calculated.

22
Characteristic Requirements:

The pressure of gases increases rapidly when the sample burns in

the bomb, the bomb walls, lid and joints should be strong enough to with
stand the maximum working pressures and there should be no leaks.
Normal working pressures are above 30 atmospheres and overload
pressures peak up to 100 atmospheres.

The capacity of the bomb should be large enough to store enough

oxygen to ensure complete burning of the sample.

During burning the nitrogen & sulfur contents are oxidized to gases
and then to nitric acid. The bomb lining must therefore be resistant to
acidic and should be corrosion free.

The stirrer unit should not generate heat due to stirring; otherwise
the calculations will lead to erroneous results.

All surfaces should have high reflectance to minimize radiation

losses.

Water equivalent of the calorimeter assembly should be small to

ensure maximum rise in temp of water following ignition.

23
Figure 2.5 Bomb Calorimeter and its accessories

24
Figure 2.6 Schematic diagram of the Bomb Calorimeter

25
Figure 2.7 Block Diagram to connect ignition wire cotton thread and sample

1. Bomb Lid-Stand
2. Stand Bracket Adjusting Screw
3. Stand Bracket
4. Bomb Lid
5. Crucible holding Electrode
6. Smaller Electrode
7. Ignition Wire Lightening holder
8. Crucible Holder Adjusting Screw
9. Crucible
10. Sample
11. Cotton Thread
12. Ignition Wire

26
 Figure 2.8 Block Diagram of oxygen filling in Bomb with safety device

1. Oxygen cylinder
2. Fine regulating Valve (For Oxygen)
3. Copper tube connect oxygen cylinder & pressure gauge
4. Pressure gauge
5. Copper tube to connect pressure gauge & bomb
6. Coupling nut with bomb
7. “O” ring
8. Bomb valve
9. Bomb body
10. Safety device

27
 The mixed biomass fuel samples prepared are palletized using hand
Pelletier. No separate binder is used. The moisture content present in the
samples acts as the binder. Immediately after palletizing a portion of the
pellet is transformed in to the crucible.

Similarly the charred biomass samples are ground once again using
mortar and chisel to get fine powder. This powder is then palletized and
used. For all the desired combinations of the samples the same procedure
is followed and the calorific values are determined.

Using suitable conversion formulae the values are represented in K

cal/Kg & MJ/Kg.

2.4.6 Flammability Apparatus:

The apparatus used for measuring the flammability index was

designed by the biomass characterization study group at MHD, BHEL
Trichy lead by Dr. A. Lawrence. The apparatus thus designed is based on
the one developed by Godbert at the Sheffield Laboratories of the British
Safety-mines Research board and subsequently refined by Finney and
Spices. A Schematic diagram of the apparatus is shown in Figure 2.9.

The storage reservoir for O2 was constructed from a two liter flask
and was connected by means of 10mm glass tubing to a suitable mercury
reservoir cum manometer as well as to oxygen reservoir was attached to a
solenoid valve by means of rubber tubing. The outlet solenoid value was
connected to glass connecting piece.

28
Figure 2.9 Schematic Diagram of Flammability Apparatus

29
 This glass connecting piece was designed in such a way that a semi
cylindrical boat like arrangement was made, into which the fuel sample
could easily and conveniently be placed for insertion in to the horizontal
arm of the ignition tube. The ignition tube was constructed wholly of
Pyrex glass and the fitted in to the stainless steel linear of 250mm high
electrically heated furnace. Temperature control was obtained by sensing
the inner wall of the ignition tube by means of a chrome-alumel
thermocouple which was connected to a temperature controller.

Visual temperature indication was continuous and any temperature

between ambient and 950˚C could be obtained. The measurement of
exact temperature of the order of ±1˚C of the ignition tube at any
particular point could be measured by sensitive thermometer.

2.4.7 Thermo Gravimetric Analyzer (TGA):

In this technique the change in sample weight is measured while

the sample is heated at a constant rate (or at constant temperature), under
air (oxidative) or nitrogen (inert) atmosphere. This technique is effective
for quantitative analysis of thermal reactions that are accompanied by
mass changes, such as evaporation, decomposition, gas absorption, and
dehydration. The simplified diagram for the instrumentation is given as
Figure 2.10.

30
 The micro-balance plays a significant role .During measurement
the change in sample mass affects the equilibrium of the balance. This
imbalance is fed back to a force coil, which generates additional
electromagnetic force to recover equilibrium. The amount of additional
electromagnetic force is proportional to the mass change. During the
heating process the temperature may go as high as 1500˚C inside the
furnace. The photographs of the Thermo Gravimetric Analyzer are given
as Figure 2.11.

FIGURE 2.10. Thermo gravimetric Analyzer

31
Figure 2.11 Thermo Gravimetric Analyzer

32
2.4.8 Differential Thermal Analysis (DTA):

This technique measures the temperature difference between a

sample and a reference material as a function of temperature as they are
heated or cooled or kept at a constant temperature (isothermal). Here the
sample and reference material are simultaneously heated or cooled at a
constant rate. Reaction or transition temperatures are then measured as a
function of the temperature difference between the sample and the
reference. It provides vital information of the materials regarding their
endothermic and exothermic behavior at high temperatures. It finds most
of its applications in analyzing and characterizing clay materials, ceramic,
ores, etc.

2.4.9 Scanning Electron Microscopy (SEM):

The principle used in this technique is as follows: when an electron

beam is focused onto the sample surface kept in a vacuum by electro-
magnetic lenses (since electron possesses dual nature with properties of
both particle and wave an electron beam can be focused or condensed like
an ordinary light). The beam is then scanned over the surface of the
sample. The scattered electron from the sample is then fed to the detector
and then to a cathode ray tube through an amplifier, where the images are
formed, which gives the information on the surface of the sample. The
simplified diagram for the instrumentation is given as Figure 2.12.

The instrument comprises of a heated filament as source of electron

beam, condenser lenses, aperture, evacuated chamber for placing the
sample, electron detector, amplifier, CRT with image forming electronics,
etc.

33
 FIGURE 2.12. Block diagram of Scanning Electron Microscope

This Scanning electron microscopy has been applied to the surface

studies of metals, ceramics, polymers, composites and biological
materials for both topography as well as compositional analysis.

2.5 Measurements for host materials

In order to carry out the detailed characterization of the bio residue
mixtures initially such characterization was carried out for the host
materials to prepare the baseline for our further studies. For this we need
to standardize and systemize our measurements. Such results are now
available in literature from a host of earlier work done.

34
 A comparison of our results with the available literature gives us
the confidence and reliability limits. Now we present our results for the
characterization of the three host materials, namely rice husk, saw dust
and ground nut shell.

2.5.1 Bulk density Determination:

For finding the bulk density of all samples the simple formula used
is given below:

Mass of the sample taken

Bulk density = Kg/m3
Volume of the sample taken

For measuring the mass of the sample the electronic balance Adair
Dutt Ad-60B was used. The samples of 300 micron size were used and
50gms of accurate measured sample was used to find the volume by using
Quanta chrome make Dual Auto Tap Model.

The sample was poured in to the measuring cylinder of 100ml

capacity (unit ±0.1 ml accuracy) and placed on one side of the tap.
Similarly sample was placed on the other side of the tap as a duplicate
sample. The number of tapping needed is set as 1000 and the equipment
was started. The cylinders went around rotary motion and also tap
motions.

When the present 1000 tapping were over the cylinders with
settled samples were taken out the volume occupied by the actual sample
was noted knowing the weight and volume of the sample its bulk density
was determined. The same procedure is used for finding the bulk density
of all the samples.

35
2.5.2 Proximate Analysis:

Proximate analysis involved the determination of moisture content,

volatile matter, ash content and fixed carbon. Proximate analysis provides
valuable information in assessing the quality of the fuel source. For
carrying out the proximate analysis of bio residue the ASTM standards
ASTM D3172-73 through D3173-75 are used (Grover et al 1989)

a) Moisture content determination:

About 15g of finely powdered air-dried sample was weighed in a

crucible. The crucible was than placed inside an electric furnace like
muffle furnace maintained at 105˚C to 110˚C. The crucible was allowed
to remain in the furnace for approximately 40 minutes until constant
weight was obtained. Then the crucible was taken out using a pair of
tongs, cooled and weighed. Loss of weight is reported as moisture on
percentage basis. (Jain & Jain, 1998)

Moisture % = (loss of weight of the sample/weight of the sample

taken) ×100

By this method the moisture content of the first host material, rice
husk is determined. The Moisture content of RH is 10.78%. The studies
made by Mohamad Yusof et al (2008) give the moisture content of rice
husk as 10.40%. Lawerence.A reported in his thesis (1999) the Moisture
content of RH sample he used as 8.38%.

The study made by Maharaj Narain (1999) gave the Moisture

content of the rice husk obtained from different varieties of Indian paddy
as IR8-8.87% Patnai-10.38% Padma-6.62% , Dular 10.50% & Basmati-
6.16%. These references support our present value of 10.78% well. They
also confirm the fact that moisture content of a bio residue varies
36
depending on the variety of the rice and on the climate conditions of the
location from which the rice husk samples are collected.

The moisture content measured by us for our second host material

saw dust is 18.34%. The result in the study of cyclone gasifiers by
Mohamad Yusof et al (2008) shows the Moisture content of SD as 12-
90%. Thesis by Lawerence (1999) reports the value as 9.35%.

For our third host material ground nut shell the moisture content
measured is 8.38%.This value is highly coinciding with the work done by
Bhoi et al (2006).The value of Moisture content of ground nut shell
reported by them is 8%. The analysis of agricultural residues done by
Werther et al (2000) indicates the moisture content of ground nut shell as
7.88%. The literature survey listed above for the three host materials
supports the values of the moisture content we have measured.

b) Volatile matter determination:

The sample left out in the crucible after moisture determination

was then covered with a lid and placed in the muffle furnace now
maintained 600˚ C for 6 minutes & then at 900˚ C for another 6 minutes.
The crucible was first air cooled and then placed inside desiccators and
weighed of air. Loss in weight was reported as volatile matter on
percentage basis. (Jain & Jain (1998) and Grover Et al (1989)).

Volatile matter % = (loss in weight due to removal of volatile/

weight of sample taken) × 100

The volatile matter determination is based on the ASTM standards

D3172-73 through D3173-75, modified procedures recommended for

37
volatiles. The volatile matter thus determined for our rice husk sample is
55.52 %.

The results given by Lawerence et al (2001) reported the volatile

matter of rice husk as 62.32%. Grover et al (1988) gave the VM of their
rice husk sample as 60.64% Mohamad Yusf et al (2008) in their studies
presented the volatile matter of RH as 62.95 %.

The Volatile matter measured for the second host material saw dust
is 65.07%.While searching the literature we are able to get similar results
to support our result. Kati Savolaiven (2008) in his studies on co-firing of
bio mass in coal-fired utility boilers reports the VM of saw dust as 85-
87%.

The volatile matter for the third host material ground nut shell is
63.81%. Bhoi et al (2006) gave the volatile matter of GS as 82.7% on dry
basis. Werther et al (2006) in their study on combustion of agricultural
residues presented the volatile matter of GS as 68.1 %. Grover et al
(1988) reported the volatile matter for GS as 68.12 %

c) Ash Content:

The next important parameter in the proximate analysis is ash

content of the bio residues. For the host materials the ash content is
determined as per ASTM standards D3172-73 through D3173-75. The
sample left out after studying volatile matter is kept at a temperature of
750˚ C in the muffle furnace for a period of two hours or more till
constant weight is recorded. The weight of the residue left out is the ash
content of the bio mass.

38
 The ash content of the RH sample is 17.36%. Among the three host
materials chosen (RH, SD, GS) the RH is having high ash content.
Because of this high ash content RH has adverse flow properties and it is
one of the difficult bio mass residues for gasifiers. Grover et al (1989)
reported the ash content of RH as 19.5%. According to Mohamad Yusuf
et al (2008) the ash content of the RH sample is 18.15 %. The
experimental research on RH combustion carried out by Chen Guanyi et
al (1997) reports the ash content of RH as 16.92%. Lawrence
(thesis1999) in his thesis gave the ash content of the RH sample he used
as 14.92%.

The ash content of SD sample is the lowest of the 3 host materials

& it is only 3.42%. The ash content of SD used by Lawerence (Thesis
1999) is only 1.79%. Bo Leckner(1998) reported in his research paper the
ash content of saw dust of different trees as ranging from 3 to 4 %

The ash content determined for the third host material ground nut
shell comes out as 5.41% whereas the results given by Werther et al
(2000) showed the ash content as 3.1%. The value reported by Lawrence
(Thesis,1999) is 5.48%. Grover et al (1989) in their work established the
ash content of GN Shell as 6.9 %

d) Fixed Carbon:

The fixed carbon content is found by applying the mass balance for
the bio residues. The fixed carbon by difference is calculated using the
formula.

Fixed carbon % = 100- (MC % +VM% +Ash content %)

39
 The fixed carbon content of any fuel is one of the most important
parameters used in determining the efficiency of fuel burning equipments.
The burning of fixed carbon is the rate determining step for the overall
combustion and fixed carbon content influences the design of burning
apparatus.

The fixed carbon content calculated by using the formula given

above for the 3 host materials RH, SD & GS is 15.34% 15.30% &
22.40% respectively. While comparing these values with Lawerence
(Thesis 1999) it is noted that the FC values calculated for RH, SD& GS
samples used by him were 14.38%, 19.55% & 19.36% respectively. The
reports given by Grover et al (1988) gave the FC values as 19.99% for
RH, 25 % for GS.

Bhoi et al gave the fixed carbon of GS as 11.73 % Werther et al

(2000) in their analysis of combustion of agricultural residues gave the
FC content of ground nut shell as 20.9 %. Bo Leckner (1998) in his
research paper reported the FC of SD as varying from 13% to 19 %.

The proximate analysis done for the three host materials agree very
well with the proximate analysis results of the same three bio residues
available in the literature . This shows the reliability and standard of the
procedure we followed to do the proximate analysis of the materials.

Ultimate Analysis:

The ultimate analysis gives C, H2, O2, N2, S and other contents of
the fuel. Since N2 &S are normally negligible C, H & O content are
important. C-H-O analysis is done by ASTM standards. The
determination of C, H2, N2 is based on ASTM-3174-76. The
determination of C, H2, and N2 were carried out simultaneously using

40
CHN-elemental analyzer. A weighed quantity of the same was burnt in
pure oxygen at 950˚C. Then the CO2, water vapors, oxides of N2 and
oxides of sulfur were the possible products of combustion.

Oxides of sulfur were removed with Calcium Oxide in the

secondary combustion zone so that water vapor cannot combine to form
sulfuric acid.

The remaining gases of combustion were collected in a ballast

volume and were allowed to mix thoroughly. For the N2 determination a
10cc aliquot was taken. The aliquot was carried by Helium in a reagent
train consisting of hot Cu and N-catalyst for the removal of O2 and the
reduction of NO to N2, sodium hydroxide for the removal of CO2 and
magnesium per chlorate for the removal of H2O.

The remaining elemental N2 was measured by the thermal

conductivity cell. Simultaneous to N2 measurement, the C & H2 infrared
cell measures CO2 and H2O levels. The infrared cell outputs were
linearized (thermal conductivity cell was already linear) and all the
outputs were multiplied by the appropriate calibration factor.
Subsequently, adjustments were made for blank and weight
compensation. When these calculations were complete, the results of the
three elements were displayed in weight percent. Using air dried moisture
content of the bio mass fuel samples the results were also calculated on a
dry basis.

41
a) Determination of Sulfur:

The total sulfur in a bio mass sample was determined as per ASTM
D 3177 “The sulfur analysis in the samples of coal and coke method A-
Eschka Method”.

The sample was ignited in intimate contact with Eschka C2 parts by

weight of magnesium oxide ±1 part by weight of sodium carbonate. The
soluble sulfur compounds were leached out and oxidized with bromine to
form sulfates, followed by acidification and precipitation as Barium
Sulfate which was filtered, ignited and weighed.

b) Determination of Oxygen:

The percentage of oxygen was calculated as per ASTM procedure

by subtracting the sum of the other components of ultimate analysis viz,
carbon, hydrogen, nitrogen, sulfur, ash and moisture from 100.

Oxygen %=100-[C% +H2% N2% +S% + Ash% + Moisture%]

Comparison of Ultimate Analysis results with literature:

a) Ultimate Analysis of Rice husk:

For the first material Rice husk, the ultimate analysis values
obtained are C=32.46%, H2=4.18%, N2=0.66%,S=0.06% and O2=34.3%

Comparing these values with values reported by Mohamad Yusof

et al (2008) we get C=37.85%, H2=5.2%, N2=0.14%, S=0.61% and
O2=27.65%.

The ultimate analysis of RH presented by Chen Guanji et al (1997)

is as follows C=37.6 %, H2=5.776%, N2=1.88% S=0.094% O2=37.62%.

42
 The data available in Lawrence thesis (1999) with regard to
ultimate analysis of RH is C=35.23 %, H2=4.38%, N2=0.7% S=0.09%
O2=36.30%.

All these referred values have agreed very well with the results
obtained by us.

b) Ultimate Analysis of Saw Dust:

The results of the ultimate analysis of the second host material SD

are C=40.17%, H2=4.9, N2=0.49%, S=0.19% & O2=32.56 %

Lawrence (Thesis 1999) shows these values as C=43.88%,

H2=5.14%, N2=0.45%, S=0.20% & O2=39.14 %. Bo Leckner (1998)
reported the ultimate analysis of SD as C = 50.54%, H2 = 5-6%, N2 =
0.03-1.08%, S = 0.01-0.11% & O2 = 39-44 %

c) Ultimate Analysis of Ground nut Shell:

The elemental analysis of Ground nut shell gives the result as

C=43.92%, H2=5.08%, N2=1.28%, S=0.12% & O2=35.81 %

Comparing these values with values available from Lawrence

(thesis 1999) we get C=42.66%, H2=5.00%, N2=1.22%, S=0.14% &
O2=36.81 %.

Werther et al (2006) reported the ultimate analysis of GS as

C=50.9%, H2=7.5%, N2=1.2%, S=0.02% & O2=40.4 %

Ayhan Demirbas (1999) reports the ultimate analysis of GS as

C=47-53%, H2=5.7-6.5%, N2=0.1-0.5%, S<0.1% & O2=39-44 %

43
 It is noted that the ultimate analysis values of the literature coincide
with the results obtained from the present study. This gives conformity of
the methodology and procedure followed by us.

2.6 Conclusion:
In this chapter we have briefly described the methods of preparing
the samples along with a discussion on the instruments used.

The proximate analysis and ultimate analysis of the three host

materials used are also discussed by comparing our results with those of
earlier workers. This study thus gave us the basic foundation of utilizing
our results of the host materials with confidence. It is to be mentioned
that the present results are in reasonable agreement with those in the
literature with in the limits of errors that may arise as a result of local
nature of the samples used.

44