CHAPTER THREE

3.0 EXPERIMENTAL METHOD

3.1 MATERIALS USED

The raw materials rice husk was collected from a local Rice Processing
Mill Ebute Ajebo Road, Imota Lagos state and sawdust was collected
from Itamaga Sawmill, Ikorodu, Lagos State.

The textile effluent was collected from Nichemtex Textile Limited, Ibeshe
Ebute Road, Lagos state.

Distilled water and other reagents used such as phosphoric acid was
gotten from chemical market, Ojota.

3.2 EQUIPMENT USED

The equipments that were used in this experiment includes:

Beakers, conical flasks, pH meter, HI96107 pH, Uv – viable

spectrophotometer, 6405 uv/vs, filter paper, sieves of size 300, 150 and
600 microns, furnance, weighing balance ATOM A – 110C, FTIR
Spectrophotometer, Dissolved Oxygen Meter, Stirrer, Thermometer, Stop
watch, Pestle and Mortar, conductivity meter (Mettler T650)

3.3 PREPARATION OF ADSORBENTS

Rice husk was soaked in distilled water to three days and washed
severally with clean water until all the colour extract was removed until
clean water was obtained. It was dried in a furnace for 2 hours at 200 0C.
20g of dried rice husk was weighed into 0.02 molar concentrated phonic
acid for 24 hours. The rice husk from the chemical was removed by
filtration and was dried in furnace at 1000C for 10 minutes.

The chemically activated carbon from rice husk was stored in a clean
plastic container prior to use for adsorption study.

15
 Sawdust was washed with distilled water to remove any impurities such
as dust. It was then dried in furnace for 3 hours at 300 0C. 20g of activated
sawdust was weighted into 0.02 molar concentration of phosphoric acid
for 12hours for chemical activation.

It was removed by filtration and put in the furnace for 30 minutes at

1000C. The chemically activated carbon from sawdust was stored in a
clean container prior to use for adsorption study.

The prepared chemically activated carbon from both rice husk and
sawdust were sieved using mesh size of 150, 300 and 600 microns and
were stored separately.

3.4 ADSORPTION EXPERIMENT

In four conical flasks, 100ml of textile effluents were taken and 3g (300
microns) of rice husk and sawdust activated carbon was weighed and
added to 2 conical flasks.

8g (300 micron) of rice husk and sawdust activated carbon were also
added to the other two conical flasks.

Conical flasks were then subjected to mixing on a magnetic stimer for

predefined maximum adsorption time 60 minutes and at 40 0C
temperature.

This procedure was repeated 8g (150 microns) and 16g (150 microns) of
both activated rice husk and activated sawdust varying the pH and
temperature

3.5 ANALYSIS

16
 Adsorbents were removed by filtration in order to get the clear samples.
Uv – visible spectrophotometer was used for measuring percentage
transmittance for determining the solution concentration.

Dissolved oxygen meter was also used to measure the total dissolved
oxygen.

All other physico – chemical parameters were measured as per standard

and methods.

The quantity of dye stuff retained on activated carbon phase was

calculated using

(C O C t )
q t

1000 M
v ………………………………………………(1)

Where Co and Ct are initial and final concentration of textile effluent

respectively, v is the volume (ml) and M is mass (g) of the activated
carbon

The percentage removal of the dye is given by:

(C O C t)
% Re moval  100
…………………………………….(2)
c o

3.6 ADSORPTION ISOTHERMS:

Equilibrium analysis, of adsorption process was carried out by using
linearized Langmuir and Freudlich models respectively equations.

1 1 1 1
  …………………………………………..(3)
q o
q m
q c
mkL e

17
 1
Ln ( q )  Lnk f

n
ln(ce) ………………………………………….

(4)

3.7 CHEMICAL CHARACTERIZATION OF ACTIVATED CARBON

Characterization of Activated Carbon

The surface functional group of activated carbon samples were identified

by Fourier transform infrared spectrophotometer using an IR prestige 21,
operating in range of 4000 – 500cm -1 and employing the KBr pellet
method.

3.8 PHYSICAL CHARACTERIZATION

1. Carbon yield: The total yield were determined after sample processing in
terms of raw material mass.
w
y   100
c
w0

Yc – carbon yield (%), W is dried weight of activated carbon prepared and

wo is the pretreated sample used in the carbonization and activation
process.

2. pH and conductivity: 1g of activated carbon was weighed and transferred

into a beaker. 100ml of distilled water was measured and added stirred for
1 hour. The samples were allowed to stabilize before the pH was
measured. The pH was determined using pH meter and conductivity was
taken using a conductivity meter at room temperature.
3. Solubility in water: 0.5g of activated carbon samples were added to
100ml of distilled water in 250ml flasks and shaked vigorously on a
magnetic shaker for 2 hours at ambient temperature. The mixture was
filtered using filter paper, the residue on filter paper was dried in an oven.
After 100mg to ambient temp, the filter paper together with residual

18
 carbon were weighted. The percentage solubility in water was calculated
as the weight rate of unrecovered carbon to the original sample:
Loss in weight on dissolution
%S   100
weight of original carbon

4. Moisture content: 1g of air dried activated carbon powder was taken in a

crucible and placed in an oven maintained at 110 0C for 1 hour. Then it
was taken out, cooled and weighed again. The loss in weight of activated
carbon in percentage gives the moisture content of the sample:
Loss in weight on drying
Moisture %   100
initial sample weight

5. Ash content: The activated carbon sample was heated at 6500C for several
hours until constant weight has been achieved. The ash was the weighed
D-B
and ash content was calculated as: Total ash %   100
C-B

B – is the weight of crucible (g)

C – is the weight of crucible plus original sample (g)

D – is weight of crucible plus ash containing sample (g)

6. Determination of density: An empty dry cylinder was weighed. A sample

of dry activated carbon were packed into the cylinder and reweighed.
3 weight of dry activated carbon
Density (g/cm) 
volume of dry materials

19
 CHAPTER FOUR
4.0 RESULT AND DISCUSSION
Removal efficiency (%)
Removal efficiency of waste water was calculated using the equation below:
Removal efficiency = (Co - Ct) × 100

Co
Where Co is initial concentration and Ct is the concentration of waste water after
adsorption for a period of time.

4.1 USING 100ml TEXTILE EFFLUENT

TABLE 1: PRESENT DATA ON EFFECT OF TIME USING ACTIVATED
RICE HUSK
Time Ct (Co - Ct) (Co - Ct) (Co - Ct) ×100
(mins) (mg/l) (mg/l) Co Co
10 15.11 14.94 0.497 49.70
20 10.21 19.84 0.660 66.00
30 5.50 24.55 0.816 81.60

40 1.21 28.84 0.960 96.00

Initial concentration = 30.05mg/l

20
FIGURE 1: Effect of contact time with constant dosage (3g), particle size
(300mic)and volume of adsorbate (100ml)on adsorbent effect for rice husk
activated carbon.

TABLE 2: PRESENT DATA ON EFFECT OF TIME USING SAWDUST

ACTIVATED CARBON.
Time Ct (Co - Ct) (Co - Ct) (Co - Ct) ×100
(mins) (mg/l) (mg/l) Co Co

10 20.11 09.94 0.330 33.00

20 16.24 13.81 0.459 45.95
30 08.33 21.72 0.722 72.27
40 02.10 27.95 0.930 93.30
Initial concentration = 30.05mg/l

FIGURE 2: Effect of contact time with constant dosage (3g), particle size
(300mic) and volume of adsorbate (100ml) on adsorbent effect for sawdust
activated carbon.
TABLE 3: DOSAGE EFFECT USING ACTIVATED RICE HUSK

21
Mass Cg (Co – Cg) (Co – Cg) (Co – Cg)×100
(g) (mg/l) (mg/l) Co Co

2 4.86 25.19 0.83 87.00

4 2.23 27.82 0.925 92.50
6 1.010 29.04 0.966 96.60
8 0.89 29.16 0.970 97.00
Initial concentration = 30.05mg/l

FIGURE 3: Effect of dosage with constant particle size 300mic), time

20mins), and volume of adsorbate (100ml) on adsorbent effect for rice husk
activated carbon.

TABLE4: DOSAGE EFFECT USING SAWDUST ACTIVATED CARBON.

Mass Cg (Co – Cg) (Co – Cg) (Co – Cg)×100
(g) (mg/l) (mg/l) Co Co

2 4.95 25 .1 0.835 83.50

4 3.54 26.51 0.882 88.20
6 2.33 27.72 0.922 92.20
8 0.99 29.06 0.967 96.70
Initial concentration = 30.05mg/l

22
FIGURE 4: Effect of dosage with constant particle size (300mic), time
(20mins), and volume of adsorbate (100ml) on adsorbent effect for sawdust
activated carbon.
TABLE 5: PRESENT DATA ON EFFECT OF TEMPERATURE USING
RICE HISK ACTIVATED CARBON.
Temperature Ct (Co - Ct) (Co - Ct) (Co - Ct) ×100
(oC) (mg/l) (mg/l) Co Co
40 7.32 22.73 0.756 75.60
50 5.43 24.62 0.819 81.90
60 4.32 25.73 0.856 85.60
70 2.20 27.85 0.926 92.60
80 1.10 28.95 0.963 96.30
Initial concentration = 30.05mg/l

23
FIGURE 5: Effect of temperature with constant particle size (150mic),
dosage (8g), time (20) and volume of adsorbate (100ml) on adsorbent effect
for rice husk activated carbon.

TABLE 6: PRESENT DATA ON EFFECT OF TEMPERATURE USING

SAWDUST ACTIVATED CARBON.
Temperature Ct (Co - Ct) (Co - Ct) (Co - Ct) ×100
(oC) (mg/l) (mg/l) Co Co

40 4.320 25.730 0.856 85.600

50 3.910 26.140 0.869 86.900
60 2.490 27.560 0.915 91.500
70 1.090 28.960 0.963 96.300
80 0.900 29.150 0.970 97.000
Initial concentration = 30.05mg/l

24
FIGURE 6: Effect of temperature with constant particle size (150mic),
dosage (8g), time (20mins) and volume of adsorbate (100ml) on adsorbent
effect for sawdust activated carbon.

TABLE 7: PRESENT DATA ON EFFECT OF pH USING RICE HUSK

ACTIVATED CARBON
pH Ct (Co - Ct) (Co - Ct) (Co - Ct) ×100
(mg/l) (mg/l) Co Co
1 1.075 28.975 0.9642 96.420
3 0.837 29.213 0.9721 97.210
5 0.120 29.939 0.9960 99.600
6 0.745 29.305 0.9700 97.520
7 0.945 29.105 0.9685 96.850
Initial concentration = 30.05mg/l

25
FIGURE 7: Effect of pH with constant particle size (150mic), dosage (g),
time (20mins) and volume of adsorbate (100ml) on adsorbent effect for rice
husk activated carbon.
TABLE8: PRESENT DATA ON EFFECT OF pH USING SAWDUST
ACTIVATED CARBON.
pH Ct (Co - Ct) (Co - Ct) (Co - Ct) ×100
(mg/l) (mg/l) Co Co
1 0.890 21.160 0.977 97.700
3 0.614 29.436 0.984 98.400
5 0.051 29.999 0.997 99.700
6 0.631 38.030 0.984 98.400
7 0.792 37.458 0.979 97.900
Initial concentration = 30.05mg/l

26
FIGURE 8: Effect of pHwith constant particle size (1.18mm), dosage (16g),
time (20mins) and volume of adsorbate (100ml) on adsorbent effect for
sawdust activated carbon.

4.2ISOTHERM MODEL
Equilibrium data commonly known as adsorption isotherm, are basic
requirements for the design of adsorption system (Ozer and Dursan, 2007). The
equilibrium data were modelled with the Langmuir and freundlich model.

4.2.1LANGMUIR ISOTHERM
RICE HUSK ACTIVATED CARBON
The amount of adsorption at equilibrium, qe (mg/l) is calculated as follows
qe =(Co – Ct) V
W

Where Co and Ct are the liquid phase concentration at initial and equilibrium,
V (L) = volume of the solution, W (g) = mass of dry adsorbent used, y =
concentration of contaminant absorbed (mg/l).
At 2g

27
qe = 25.19 = 12.595mg/l
2
TABLE 11: LANGMUIR ISOTHERM FOR RICE HUSK ACTIVATED
CARBON
Mass Cg(mg/l) Co- Cg qe 1 1
(g) (mg/l) qe Cg
2 4.864 25.19 12.595 0.0813 0.206
4 2.231 27.82 6.995 0.1437 0.448
6 1.010 29.04 4.840 0.2066 0.990
8 0.896 29.16 3.645 0.2743 1.116
Initial concentration = 30.05mg/l

FIGURE 11:
The linear
plot of
specific
adsorption
against the
equilibrium concentration.
From the graph plotted
Slope = 0.034
Intercept = 0.009
Correlation coefficient (R2) = 0.963
Calculating for qm and ka from the linear equation of Langmuir isotherm
1/ qe = 1/ka+ 1/qm
where 1/ qm = intercept
= 0.009
Also 1/ ka= slope
= 0.034
The shape of the Langmuir by the dimensionless constant separation term (RL)
to determine high affinity adsorption and is expressed as
28
RL = 1/1+ kaCt
RL = 0.947

TABLE 12: LANGMUIR ISOTHERM FOR SAWDUST ACTIVATED

CARBON
Mass Cg(mg/l) Co- Cg qe 1 1
(g) (mg/l) qe Cg
2 4.95 25.10 12.55 0.0796 0.2020
4 3.54 26.51 6.6275 0.1508 0.2124
6 2.33 27.72 4.6200 0.2164 0.4291
8 0.99 29.06 3.6325 0.2752 1.010
Initial concentration = 30.05mg/l

FIGURE 12: The linear plot of specific adsorption against the equilibrium
concentration.
From the graph plotted
Slope = 0.008
Intercept =0.022
Correlation coefficient (R2) = 0.792
Calculating for qm and ka from the linear equation of Langmuir isotherm
1/ qe = 1/ka+ 1/qm
where 1/ qm = intercept

29
 = 0.022
Also 1/ ka= slope
= 0.008
The shape of the Langmuir by the dimensionless constant separation term (RL)
to determine high affinity adsorption and is expressed as
RL = 1/qe + kaCt
RL = 0.955.

4.2.2 FREUNDLICH ISOTHERM

RICE HUSK ACTIVATED CARBON
The equilibrium data were analyzed using linear form of Freundlich isotherm by
plotting log qe versus log Ct, M (g) mass of adsorbent, X (g) mass of adsorbate
and Ct(mg/l) equilibrium concentration.
TABLE 13: FREUNDLICH ISOTHERM FOR RICE HUSK ACTIVATED
CARBON
Mass Cg(mg/l) Co- Cg qe log qe log Cg
(g) (mg/l)
2 4.864 25.19 12.595 1.001 0.6820
4 2.231 27.82 6.995 0.8422 0.3483
6 1.010 29.04 4.840 0.6848 0.3213
8 0.896 29.16 3.645 0.5616 0.0505
Initial concentration = 30.05mg/l

30
FIGURE 13: Linear graph of log qe against log Cg.
Slope = 0.689
Intercept =1.337
Correlation coefficient (R2)= 0.981
Calculating for kfand n from the linear form of Freundlich equation
Log qe = log kf + 1/n logCe
1/n = slope
n = 0.978
kf= 0.168

TABLE 14: FREUNDLICH ISOTHERM FOR SAWDUST ACTIVATED

CARBON
Mass Cg(mg/l) Co- Cg qe log qe log Cg
(g) (mg/l)
2 4.95 25.10 12.55 1.098 0.694
4 3.54 26.51 6.6275 0.8213 0.549
6 2.33 27.72 4.6200 0.6646 0.3610
8 0.99 29.06 3.6325 0.5602 0.0043
Initial concentration = 30.05mg/l

31
FIGURE 14: Linear graph of log qe against log Cg.
Graph of log qe against log Cg from the graph plotted
Slope =0.553
Intercept =1.517
Correlating coefficient =0.875
Calculating for kfand n from the linear form of Freundlich equation
Log qe = log kf + 1/n logCe
1/n = slope
n = 0.957
kf= 0.919

4.3 Table 15: Physical Characteristics of Rick Husk activated Carbon and Sawdust activated
Carbon
32
PARAMETERS RICE ACTIVATED SAWDUST
CARBON (RAC) ACTIVATED
CARBON (SAC)
Carbon yield (%) 29.4 32.8
pH (1% solution) 6.10 7.30
-
Conductivity (μScm 326.50 144.01
1
)
Solubility in water 8.4 6.7
(%)
Density (gcm-3) 0.58 0.45
Moisture content (%) 95.60 5.40
Ash content (%) 6.60 6.80

Characterization of the carbon is important in the formulation of a

consistent quality carbon that can be used in water treatment plants or any
other industreial applications. The physical characteristics of the prepared
carbons are listed in table 1. The carbon yield for RAC is 29.4% while
SAC is 32.8%.

These values are typical range for most activated carbon prepared from
agro waste.

As shown in Table 1 the pH values for RAC and SAC were found to be
6.10 and 7.30 respectively. The pH value is a measure of whether it is
acidic or basic. The surface of RAC was more acidic (pH = 6.0) than that
of SAC pH = 7.4.

Too high pH indicates much contamination while too low pH indicates

that acid wash was incomplete.

The electrical conductivity for RAC and SAC was 326.50 and 144.01
μscm-1 respectively. The low conductivity of SAC shows that it has very
little amount of charged and exchangeable ions.

33
Residual ionic compounds in the surface and pores are completely
washerd out which results in poor conductivity. The higher value of
electrical conductivity of RAC shows the release of additional amount of
proton CH+J having high ionic mobility and hence conductivity from the
surface of SAC.

Water solubility of RAC and SAC was determined to be 8.4% and 6.7%
respectively. Any degree of solubility in water is an indication of presence
of impurities. Pure carbon does not dissolve in water since carbon is very
unreactive due to lack of electron donating or accepting species in
structure.

Moisture content of RAC and SAC are 4.6% and 5.4% respectively.

Generally, the recommended activated carbon storage moisture content is

<3%, if the activated carbon moisture content is high, fungi and other
micro organisms degrade the carbon utilizing it in their metabolic
processes.

The micro – organism can also multiply within the micro pores blocking
the pore structure, thereby reducing the adsorptive capacity of the carbon.

High moisture content can also result from the exposure of activated
carbon to air and moisture is been absorbed from the atmosphere.

Ash content of RAC and SAC were 6.6 and 6.8% respectively. Ash
content indicates the quality of an activated carbon. It is the residue that
remains when carbonaceous portion is burned off. High ash content of
material contains high levels of impurities that lead to blockage of pores
during the activation process reducing the surface area of the activated
carbon. Low as content of RAC should impact positively on surface area
parameter.

34
 The density of 0.58g/cm3 was for RAC and 0.45g/cm3 was for SAC. The
higher the density, the better the filterability of activated carbon.

Table 16: Chemical Characteristics of Rick Husk activated Carbon

and Sawdust activated Carbon

Fourier Transformed Infrared Spectrophotometer Data of RAC and SAC

SAC RAC
Wave No. Assigned Wave No. Assigned
(cm-1) Functional group (cm-1) Functional group
3431.58 - OH 3404.58 -OH
2361.02 CH3 (Alkane 3122.95 CH3(Alkane goup)
group)
2330.16 C = C – H 2359.09 CH2
stretching
1836.35 Ar C = O 1919.29 P-O-P asymmetric
1705.18 C=C 1618.38 Stretching
1606.81 CH2 1402.34 C-P stretching
1516.15 C – H bend 1188.23 P = O stretching
1456.35 C – OH 1070.56 P – P stretching
1425.48 Secondary 962.54 Out of plane C – H
alcohols
1317.46 Primary alcohols 636.55 Bending

The qualitative characterization of surface functional groups of activated

carbon samples were performed by the FTIR technique. The results in
table 2 shows that all the FTIR spectra have similar shapes with most of
the bands located on the same wave number range.

It can be seen that increasing the intensity of the FT – IR spectra for C =

O (Carboxylic group), O-H (hydroxyl group) and C-O (Phenol group)
stretching vibrations indicate the presence more oxygen functional groups
on the phosphorized activated carbon.

35
 CHAPTER FIVE
CONCLUSION AND RECOMMENDATION

5.0 CONCLUSION
From the result obtained, it was concluded that the adsorption process is
effective in treatment of stimulated waste water. Sawdust activated carbon and
rice husk activated carbon are effective in the treatment of stimulated waste
water and economical. It is concluded when various parameters were studied to
determine the effectiveness of the adsorption of adsorbent dosage, pH, contact
36
time and temperature, rice husk activated carbon proves to be more effective
than sawdust activated carbon. The optimum adsorption capacity for adsorbent
effect for rice husk activated carbon was achieved at pH 5 and that of sawdust
activated carbon was also achieved at pH 5 when stimulated waste water was
used as adsorbate. While that of wastewater collected was achieve at pH 6 for
both adsorbents.
When Langmuir, Freundlich, Temkins isotherm model and kinetics model were
used to test the suitability of the adsorbents, it was deduced from the result
obtained that the linear plot of Temkins isotherm model gave a better fit to the
experimental data when stimulated waste water was used as adsorbate.
It was also deduced from the result obtained that the linear plot of second
pseudo order model gave a better fit to the experimental data when waste water
collected was used as adsorbate.

5.1RECOMMENDATION
It can be recommended that activated carbon produced from cocoa, banana peel,
saw dust, peanut husk charcoal, fly ash, natural zeolites, animal bone meal tea
wood bark, rice husk, cotton waste and bituminous coal can also be considered
for treatment of wastewater or industrial effluent. Also other isotherm model
such as Flory-Huggins, Hill, Dubinin– Radushkevich can also be considered in
future work.

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