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PROXIMATE ANALYSIS AND HEATING VALUE OF MARINE ALGAE

(80% BROWN ALGAE, 20% BINDER)


Special Project
Group # 9 Tamse, Jan Marvin M.
1. Introduction
1.1
This experiment aims at determining moisture content, volatile
matter, ash content, fixed carbon, and gross or higher heating value of a brown
algae.
1.2
1.3

The brown algae sample has a 20% starch as binder.


The brown algae sample was obtained from one of the shores of

Ginatilan, Cebu, Philippines.


2. Theoretical Background
2.1
Proximate analysis is the determination of the approximate overall
composition. This includes parameters such as moisture, volatile matter, ash, and
fixed carbon. All of these parameters are determined through a series of standard
test methods. Moisture, volatile matter, ash, and fixed carbon are obtained by
subjecting the fuel sample to different prescribed temperature levels for a specific
amount of time[8.1]. Then the first loss of weight is accounted to the loss of
moisture. At higher temperature, the second loss of weight is now accounted to
the loss of volatile matter. The residue after subjecting it to the final temperature
is then the ash. Finally, the fixed carbon is the difference between the sum of the
previous values and 100.
2.2
Determination of such parameters is important. Moisture, volatile
matter, and fixed carbon are used to determine the rank of a coal. Moisture
content is highest at low-rank coals. Moisture content is the percentage of the
quantity of water in the material. Determining moisture content is significant
since it affects the value of biomass fuels [8.5]. In the study of Alburo et. al.[8.6], there
is a high negative correlation between moisture content and calorific value for
ulva reticulata species but an inconsistent correlation with that of the sargassum
(brown algae). Volatile matter is an indicator of ease of ignition and also used as
basis for selling and purchasing coals[8.3].

2.3

Heating value or calorific value can be obtained using adiabatic

bomb calorimeter. It is simply the amount of energy a specific fuel will produce
during combustion. This is useful in determining the quantity of fuel to be used in
specific applications such as in boilers[8.3].
3. Material/Equipment Used
3.1
Memmert Oven used to heat sample and crucible for exactly 1
hour
3.2
3.3

Electric Furnace used to burn the volatile matter of the sample


Kern Analytical Balance used to measure the change in mass

of sample
3.4
3.5

Porcelain Crucible a 30cc crucible used to contain the sample


Desiccator sealable enclosures used to preserve moisture while

cooling
3.6

Bomb Calorimeter used to determine the gross heating value of

3.7
3.8

Ignition Unit used to control the firing of the bomb


Wiley Miller used to mill the brown algae sample

sample

Fig. 3.1 Memmert Oven

Fig. 3.2 Electric Furnace

Fig.3.3 Analytical Balance

Fig. 3.6 Crucible

Fig. 3.5 Desiccator

Fig. 3.6 Bomb

Fig. 3.7 Ignition Unit

4. Methodology
4.1
Proximate Analysis
4.1.1 Preparation of Samples
4.1.1.1 Brown Algae samples were sun-dried for a number
of hours in a day for 1 week.
4.1.1.2 After drying, the samples were then milled.
4.1.1.3 The samples were then mixed with starch having an
amount of 20% the total mass.
4.1.1.4 Specific samples were taken for proximate analysis
and others were briquetted, dried, and placed inside air-tight plastic
containers.
4.1.2

Constant Weight Method


4.1.2.1 The mass of a 30cc porcelain crucible was

measured using analytical balance.


4.1.2.2 The crucible was then placed inside the oven for
exactly an hour.
4.1.2.3 After, the crucible was taken out of the oven and
was placed inside the desiccator to cool it for 1 hour.
4.1.2.4 After cooling, the crucible was then placed inside
the analytical balance to measure the change in weight.
4.1.2.5 When the change in weight was within .0005, the
crucible was deemed fit to continue the procedure. Otherwise, the crucible
is to be placed again inside the oven until it has a constant weight.
4.1.3 Determination of Moisture
4.1.3.1 1 gram of brown algae sample having 20% binder
as prepared was weighed in a crucible, previously heated and cooled.
4.1.3.2 It was then placed in the oven and dried for exactly
1 hour at 104-108 C.
4.1.3.3 After drying, the crucible was then cooled in the
desiccator for an hour.
4.1.3.4 When cooled, the crucible was then immediately
weighed.

4.1.3.5 The loss of weight was recorded as the moisture and


the moisture content was then calculated.
4.1.4 Determination of Volatile Matter
4.1.4.1 The same crucible was placed inside the electric
furnace having a temperature of 950 C for exactly 7 minutes.
4.1.4.2 The crucible was then air-cooled after taking it out
of the furnace.
4.1.4.3 After, the crucible was then weighed.
4.1.4.4 The further loss of weight was then recorded as the
volatile matter and the volatile matter percentage was then calculated.
4.1.5 Determination of Ash Content
4.1.5.1 The same crucible was further heated inside the
electric furnace for an hour.
4.1.5.2 After, the crucible was cooled for a suitable amount
of time.
4.1.5.3 The crucible was then weighed and the further loss
of weight is recorded as the ash
4.1.5.4 The ash content was then calculated.
4.1.6 Determination of Fixed Carbon
4.1.6.1 To determine the fixed carbon, the remaining mass
inside the crucible was then weighed and then subtracted by the mass of
the porcelain crucible.
4.1.6.2 This value is then recorded as the fixed carbon.
4.1.6.3 This was assumed that the sample does not contain
any sulfur and thus the moisture content, volatile matter, ash, and fixed
carbon sums up to 100%.
4.2
Determination of Heating Value using Bomb Calorimeter
4.2.1 1 g of sample was placed in the cup that is to be attached on
the holders of the bomb cap.
4.2.2 A fuse wire was used to connect the electrodes found on the
bomb cap. It was placed in such a way that the wire touches the solid fuel
sample.
4.2.3

The bomb was then cap-sealed and oxygen having 25 atm

was then introduced in the bomb.


4.2.4 Wires of the ignition unit were then connected to the
corresponding holes found on the top part of the bomb cap.
4.2.5 A suitable amount of distilled water was placed in the
jacket.

4.2.6
4.2.7

The bomb was then placed in the jacket containing water.


The jacket was placed in the bomb container and was

4.2.8

The thermometer was fitted through the hole found on the

covered.
cover and the stirrer was turned on until the temperature of the water was
constant.
4.2.9

After, the stirrer was turned off and the ignition button was

pressed.
4.2.10 During ignition, the change in temperature was recorded
until it remains constant and starts to fall down.
4.2.11 After ignition, the bomb was taken out of the container and
the fuse wire was obtained.
4.2.12 The wire was then measured and the corresponding
correction for heat of combustion of firing wire, e3 was recorded.
4.2.13 The gross of heat of combustion was then computed.
5. Data and Discussion
Sample: Brown Algae (80% Algae, 20% Starch)
Table 5.1 Moisture, Volatile Matter, Ash Content and Fixed Carbon of sample
Parameters

Percentage (%)

Moisture

22.37

Volatile Matter

67.88

Ash

2.48

Fixed Carbon

7.27

CALCULATIONS:
CONSTANT WEIGHT METHOD
Equipment used: Memmert Oven
Duration: 1 hour
Table 5.2 The mass of crucible before and after subjecting it to the Memmert oven
Before Heating

After Heating

20.9738 g

20.9735 g

Since the difference between the two readings is .0003 which is within the
permissible tolerance of .0005 as stated by the chemist, the porcelain crucible now has
negligible amount of moisture and can now be used to determine the following
parameters.

MOISTURE CONTENT
Equipment Used: Memmert Oven
Duration: 1 hour
total mass = mass of crucible + mass of sample = 20.9735 g + 1 g = 21.9735 g
Table 5.3 The total mass before and after subjecting it to the Memmert oven
Before Heating

After Heating

21.9735 g

21.7463 g

The loss of weight is recorded as the moisture:


moisture content (%) =

(total mass of before heatingtotal mass after heating)


100
mass of sample
(21.9735 21.7463)
100
1

moisture content (%) = 22.37%

VOLATILE MATTER
Equipment Used: Electric Furnace
Duration: 7 minutes
Table 5.4 The total mass before and after subjecting it to the electric furnace
Before

After

21.7463 g

21.0675 g

The loss of weight is recorded as the volatile matter:


(total mass of before burningtotal mass after burning)
100
mass of sample

Volatile matter (%) =

(21.7463 21.0675)
100
1

Volatile matter (%) = 67.88%

ASH CONTENT
Equipment Used: Electric Furnace
Duration: 1 hour
Table 5.4 The total mass before and after subjecting it to the electric furnace
Before

After

21.0675 g

21.0427 g

The loss of weight is recorded as the ash:

Ash Content (%) =

(total mass of before burningtotal mass after burning)


100
mass of sample
(21.0675 21.0427)
100
1

Ash Content (%) = 2.48%

FIXED CARBON
To calculate fixed carbon easily, this equation is used:
100% = MC + VM + AC + FC

where:

MC = Moisture Content (%)


VM = Volatile Matter (%)
AC = Ash Content (%)
FC = Fixed Carbon (%)

so,

FC = 100 (MC + VM +AC) = 100 (22.37 + 67.88 + 2.48) = 100 92.73


Fixed Carbon (%) = 7.27%
The values obtained above are determined with the assumption that the remains

after ashing are considered as the fixed carbon and that the brown algae sample does not
contain any sulfur.
HIGHER HEATING VALUE
W = Hg/t

[eqn 5.1]

where: H = Heat of combustion of standard benzoic acid, 6318 cal/g


g = mass of standard benzoic acid sample
t = temperature rise
W = energy equivalent of calorimeter
for benzoic acid t = 2.7 C so,
W = (6318)(1g)/(2.7 C) = 2340 cal/ C
Sample

Temp Rise

Left Over Fuse Wire

e2

Brown Algae

.34 C

5.25 cm

2.54 cal

rearranging equation 5.1 and including correction for heat of combustion of firing wire
Gross Heat of Combustion = H = [(t)x(W) - e2] / (g)

= [ .34C x 2340 cal/C - 2.54 ]/ (1g)


= 793.6 cal

6. Conclusion
6.1

As shown in the data and discussions, moisture content, volatile

matter, ash, and fixed carbon are 22.37%, 67.88%, 2.48%, and 7.27%,
respectively. Ash content of solid fuels is preferred to be lower. The reason for
this is that an increase in the percentage of ash causes reduction to the calorific
value [8.3].
6.2

Since the calorific value and proximate analysis are used to

classify coal, it is then important to determine such parameters to that of a


biomass fuel to compare where it currently stands against coal or if it is even
feasible.
6.3
Although
7. Recommendation
7.1
It is recommended to use other test methods in determining the
fixed carbon since it was assumed in this project that the remaining amount after
ashing is simply the fixed carbon thus giving a theoretical value and not an
experimental one.
7.2
It is also recommended that a uniform drying time should be
observed otherwise it will cause an uneven moisture status or will yield different
moistures to marine algae samples.

8. Bibliography
8.1
Speight, J. (2005). Handbook of coal analysis. Hoboken, N.J.:
Wiley-Interscience.
8.2
Bloch, Heinz. Practical Lubrication For Industrial Facilities. 2nd
ed. Lilburn: The Fairmont Press, Inc, 2009.
8.3
Miller, B. and Tillman, D. (2008). Combustion engineering issues
for solid fuel systems. Amsterdam: Academic Press/Elsevier.
8.4
Rochleder, F. (1862). Proximate analysis of plants and vegetable
substances. Philadelphia: Merrihew & Thompson, Printers.