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Chapter 1

INTRODUCTION

The fast pace industrialization has become the contributing factor to the increase
in the environmental problems in our country. The use of chemicals is one of the reasons
why our environment starts to deteriorate. Organic compounds like dyes are
contaminants which are a danger to environment and to human health. It is toxic and
carcinogenic even at low concentration (El Mouzdahir, et al., 2010). Pollutants or
contaminants are seen from the wastewater of textile, paper and plastic industries.
These industries use dyes to color their product, and as a result, they produce a
coloured wastewater. The presence of dye, even in very small amount, in water is still
visible and undesirable due to its harmful effects to the environment and human beings
(Rafatullah, et al., 2010). The conventional method for dye removal are coagulation,
electrochemical processes, chemical oxidation, membrane filtration, adsorption, etc
(Weng, et al., 2007).

Adsorption is one of the most useful and effective method in removing pollutants
like organic dyes in wastewater since it is much more cost effective compared to other
methods especially if the adsorbent is inexpensive and readily available (Khaled, 2009).
Adsorption is the process of separating the constituent of a fluid by transferring it to the
surface of a solid phase which is the adsorbent (Foust, et al., 1980).

Adsorption by activated carbon is widely used in treating effluent which contains


organic dyes. Some waste materials like coir pith, coconut husk, orange peel, jackfruit
peel, etc are used as source of activated carbon (Kadirvelu, et al., 2001). These
materials are chemically modified with the use of acid or base (Prahas, et al., 2008) and
carbonized at high temperate to achieve an activated carbon (Kavitha et al., 2007).

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1.1 Statement of the Problem

The presence of dyes in wastewater is a major concern due to its harmful effects
to many forms of life. Industries such as textile, ceramic, rubber, paper, leather and
plastics, use synthetic dye as colorant for their product. The presence of even small
amounts of dyes in water (less than 1 ppm) is still visible and undesirable (Rafatullah, et
al., 2010). Dyes in effluents impede the transmission of sunlight into streams and
reduces photosynthetic activity (Garg, et al., 2004). Some industries that use dye in the
country resort in dumping their untreated effluent to water streams instead of paying or
installing expensive wastewater treatment facility.

1.2 Objectives of the Study

The purposes of the study are, first, to be able to produce activated carbon,
synthesized from breadnut peel, at different carbonization temperatures and time.
Secondly, to be able to create a correlation of percent yield, adsorption capacity, and
weight of removed pollutant per weight of dried sample with respect to carbonization
temperature and time. And from the correlation to be made, the study also aims to
estimate the optimum carbonization parameters such as temperature and time.

1.3 Importance of Study

Commercial activated carbon is expensive. Thus, manufacturing low cost yet


effective activated carbon is of great significance in wastewater treatment. In this study,
breadnut peel would be used as raw material for activated carbon.

If the optimum result can be determined, then these industries can use the
adsorption process with carbonized breadnut peel as the adsorbent for their wastewater
treatment, which can significantly reduce the cost for water treatment since the
adsorbent is a low cost, derived-waste material.

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1.4 Plan of Investigation

Breadnut peel, which is being considered as waste material in the market, is to


be collected from Nepa Q-Mart, Quezon City. The peel will be washed and dried, and to
be chemically modified by impregnating it with phosphoric acid. The chemically modified
peel will be carbonized at different temperatures and time. The produced activated
carbon will be washed, neutralized and dried. Its percent yield will be taken based on the
mass of the produced activated carbon (AC) per mass of the dried raw material.

The adsorption of Methylene Blue (MB) from aqueous solution by the AC is to be


tested by a simulation. A solution with a known concentration will be used throughout the
adsorption tests. An activated carbon with known mass will be added to a certain volume
of the MB solution, and a fixed contact time was used. The adsorption capacity of the
activated carbon was based on the mass of Methylene Blue adsorbed per mass of
activated carbon used.

1.5 Scope and Limitation of the Study

The study is limited to the use of Breadnut peel as raw material for activated
carbon by chemical activation and carbonization. The adsorption experiment only
performed in a simulated textile wastewater by introducing the produced activated
carbon in a MB solution. The study does not include the adsorption of other dyes that
are usually present in a textile wastewater, and the disposal of the activated carbon. The
parameters are the temperatures and time for carbonization. The temperatures and time
used range from 494oC to 706oC and 63 to 177 minutes, respectively. These parameters
are used as references for the determination of the optimum percent yield and
adsorption capacity for the study. Comparison in terms of effectiveness and cost
between the activated carbon produced and with what are commercially available is not
considered.

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CHAPTER 2

REVIEW OF RELATED LITERATURE

2.1 Breadnut

Breadnut (Artocarpus camansi) is a large tree, 10 to 15 meters high, similar in


habit to Artocarpus altilis. Leaves are large, leathery, ovate to oblong-ovate, 40 to 60 cm
long, 25 to 45 cm wide, with deeply incised margins, and characterized by 4- to 5-lobes.
Male spikes are cylindric, greenish-yellow, 15 to 25 cm long, and 3 to 4 cm in diameter.
Fruit is green, ovoid or somewhat rounded, up to 20 cm in diameter with a spiny surface,
with little pulp. Seeds are numerous, light brown, ovoid, rounded, about 2.5 cm in
diameter. Artocarpus species are rich in phenolic compounds including flavonoids,
stilbenoids, arylbenzofurons and Jacalin, a lectin. The fruit, particularly the young ones,
are boiled and eaten as a vegetable. While the seeds are rich in starch and could be
eaten boiled or roasted (Stuart, 2011).

Breadnut under favorable conditions can grow from 0.5–1.5 m (1.5–5 ft) in height
per year for the first 10–12 years. Mature breadnut trees in the Philippines have been
reported to produce 600–800 fruits per season. The fruiting season is October to May,
with some fruits available in July. Flowering begins in April or May in the Philippines
(Ragone, 2006).

2.2 Adsorption

Adsorption is an operation that utilizes the ability of a certain material to


concentrate specific substances from solution onto their surfaces. The components of
either gaseous or liquid can be separated in this manner.

Adsorption phenomena can be classified as physical and chemical adsorption.


Physical adsorption or van der Waals adsorption is the result of intermolecular forces of

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attraction between molecules of the solid and the substance adsorbed, which is a
reversible phenomenon. On the other hand, chemisorption or activated adsorption is the
result of chemical interaction between the solid and the adsorbed substance. The
process is frequently irreversible and the original substance on desorption would have
gone to a chemical change (Treybal, 1981).

2.3 Activated Carbon

Most dyes used in industries, especially in textile manufacturing, are designed to


be resistant to environmental conditions such as solar light, pH effects and microbial
effect. But before effluents from such industries are discharged into the environment, it is
desirable to remove these coloring-causing contaminants (Bestani, et al., 2008).

Activated carbon (AC) is commonly used as an adsorbent with proven adsorption


efficiency for organic compounds (Zhang, et al., 2009). It is a microcrystalline
(Geankoplis, 2003) and inert porous carrier material, capable of distributing chemicals
on its large hydrophobic internal surface, thus making them accessible to reactants (Yin,
et al., 2007). It is a widely used agent for refining, decolorizing, purifying or filtering
substances in varied industries (Bureau of Export Trade Promotion, 1989). Specifically,
for the removal of a wide variety of organic and inorganic pollutants dissolved in
aqueous media, or from gaseous environment (Yin, et al., 2007) due to its exceptionally
high surface areas which range from 300 to 1200 m2/g with average pore diameters of 1
to 6 nm (Geankoplis, 2003).

Easily available natural materials such as saw dust, tree barks, wool fiber, fungal
biomass, pumpkin seed hull, coconut bunch waste, broad bean peels, grass waste,
pineapple stem waste, and spent tea leaves are processed to manufacture AC because
of their renewable character, low cost and abundance (Bestani, et al., 2008; Zhang, et
al., 2009). The derivation of such waste materials has also been considered to contribute
to mitigating the problem of waste disposable (Zhang, et al., 2009). Example of materials
derived by thermal decomposition are wood chips, saw dust and coconut shells (Bureau
of Export Trade Promotion, 1989).

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Activated carbon with ample adsorption sites for molecules to attach to have
relatively high surface area and well developed porosity (Zhang, et al., 2009).
Modifications on the preparation of activated carbon for an increased effectiveness on
adsorption of organic compounds from aqueous solutions are being developed from
biomass (Yin, et al., 2007).

2.4 Methylene Blue

Methylene Blue (MB) is a cationic dye synthesized as a pure blue dye for cotton
and plays an important role in textile industry (BASF Chemical Company, 2012).

Though it is not regarded as acutely toxic, it can be harmful to the human body.
Its various harmful effects are short periods of difficulty in breathing when inhaled which
causes burning sensation, nausea, vomiting, diarrhea and gastritis when ingested
through mouth (Ozer, et al., 2007).

MB is known to have a strong adsorption onto solids. It has a molecular weight of 373.9
g/mol, which corresponds to methylene blue hydrochloride with three groups of water.
Figure 1 shows the structure of MB (Ozer, et al., 2007).

Figure 2.1. Structure of Methylene Blue

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CHAPTER 3

METHODOLOGY

3.1 Equipment

 Sartorius Analytical Balance 210S (BL210S)


 Scientific Oven 1 Series 2000
 Hitachi U-5100 UV-Vis Spectrophotometer
 Fisher Scientific Furnace
 Thermo Scientific MaxQ™ 2000 Water Bath Shaker
 Clay Adams® Compact II Centrifuge
 Orion pH 600 - pH meter

3.2 Reagents

 Dried Breadnut peels


 Distilled water
 85% (w/w) H3PO4
 Methylene Blue Dye
 0.1 M NaOH

3.3 Raw Materials Preparation

The breadnut peel was cut into pieces and washed with distilled water. After
washing, it was dried in an oven at 60 °C - 80 °C for 5 – 6 hours. The dried sample was
weighed using analytical balance. The dried sample was chemically activated using 85%
w/w H3PO4. The dried peel was placed in a beaker and was soaked in acid. It was stirred
constantly for 5 minutes for 6 hours at 30 minute interval in the fume hood. The chemical
activated sample was then dried in an oven.

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3.4 Carbonization

The chemical activated sample was placed in crucibles and was carbonized at
494-706 °C under carbonization time within one hour to three hours using a furnace.
Table 3.1 below shows the temperature and time of carbonization:

Table 3.1 Parameter Conditions

Std Run
Temp, °C Time, min
Order Order
4 1 675 160
5 2 494 120
3 3 525 160
1 4 525 80
9 5 600 120
10 6 600 120
8 7 600 177
12 8 600 120
2 9 675 80
13 10 600 120
7 11 600 63
11 12 600 120
6 13 706 120

The crucibles were cooled down in a room temperature after carbonization and
were placed in a desiccator to avoid moisture. The activated carbon was taken out from
the crucibles and was ground using mortar and pestle until fine particles of activated
carbon were achieved.

3.5 Neutralization of Activated Carbon

The activated carbon was soaked in distilled water and was stirred in a beaker. A
0.1 M NaOH was added until the pH of the mixture reached neutral level (pH 6.5-7). The
mixture was decanted when the activated carbon had settled to the bottom. The neutral
activated carbon was then dried in an oven and then weighed using analytical balance.

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3.6 Reagents / Chemicals

A 250 ppm of Methylene Blue (MB) stock solution was prepared by dissolving 0.5
grams of MB in 2000 mL of distilled water. The maximum wavelength of this dye is 664
nm (Prahas, Kartika et al., 2008).

3.7 Adsorption of Methylene Blue

A 50 mL of MB stock solution was placed in an Erlenmeyer flask followed by the


addition of 0.1 gram of activated carbon. The mixture was placed in a water-bath shaker
at 200 rpm for two hours, and then was subjected to centrifugation for 3-5 minutes to
separate the activated carbon from the solution. The carbonized samples at different
carbonization temperature and time were used to adsorb methylene blue. The
absorbance of the methylene blue solution was measured using the UV-Vis
spectrophotometer. The calibration curve was used to determine the concentration of the
solution.

3.8 Calibration Curve and Concentration

Methylene Blue solution of concentrations of 30, 25, 20, 15, 12.5, 10, 7.5, 5, and
2.5 ppm were prepared by dilution from the stock solution of 250 ppm. The absorbance
of different methylene blue solution was measured using UV-Vis Spectrophotometer at
maximum wavelength. The equipment was calibrated before measuring the absorbance
of the solution. The plot of absorbance versus concentration was used as calibration
curve to determine the final concentration. Solution with concentration exceeding 10
ppm (or its color is much darker than the color of 10 ppm solution) was to be diluted with
distilled water, and its absorbance was measured using the UV-Vis spectrophotometer.

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Chapter 4

Discussion of Data and Results

This chapter presents the analyses of the data gathered from the experiment.
Also, relevant data are presented in this chapter.

4.1 Determination of Percent Yield

Percent yield is the weight after carbonization, washing and drying divided by the
weight before activation and carbonization. The experiment showed that the lowest yield
came from the highest temperature which is 706°C with duration of 120 minutes of
carbonization. In contrast, the lowest yield gained came from the 494°C with the same
period of carbonization. Table 4.1 shows the result of the percent yield with their
corresponding time and temperature.

Table 4.1. Data of Percent Yield

wt after
wt before
carbonization,
Std Run Temp, Time, activation and %
washing & drying,
Order Order °C min carbonization, g Yield
g
4 1 675 160 5.3821 1.6006 29.74
5 2 494 120 5.844 2.0330 34.79
3 3 525 160 5.9517 1.4168 23.80
1 4 525 80 5.9492 1.5478 26.02
9 5 600 120 4.7078 1.6664 35.40
10 6 600 120 4.2552 1.6095 37.82
8 7 600 177 6.6852 2.0774 31.07
12 8 600 120 4.0609 1.8237 44.91
2 9 675 80 5.7968 1.7754 30.63
13 10 600 120 5.9743 2.2019 36.86
7 11 600 63 6.1823 1.7975 29.07
11 12 600 120 5.8068 2.3317 40.15
6 13 706 120 5.6039 1.2822 22.88

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Table 4.2 below shows the initial Minitab ® 15 response surface regression of
yield against temperature and time. The analysis was done using uncoded units.
Meaning, the estimated regression as well as the full table will only be presented.

Table 4.2. Initial Response Surface Regression: Yield versus temp, time

Estimated Regression Coefficients for Yield

Term Coef SE Coef T P


Constant -347.936 132.119 -2.634 0.034
Temp 1.165 0.400 2.915 0.022
Time 0.676 0.553 1.223 0.261
temp*temp -0.001 0.000 -3.069 0.018

-0.003 0.001 -2.728 0.029


time*time
0.000 0.001 0.138 0.894
temp*time

S = 4.79003 PRESS = 835.805


R-Sq = 68.42% R-Sq(pred) = 0.00% R-Sq(adj) = 45.86%

Analysis of Variance for Yield

Source DF Seq SS Adj SS Adj MS F


P
Regression 5 347.937 347.937 69.587 3.03
0.090
Linear 2 4.962 199.698 99.849 4.35
0.059
Square 2 342.537 342.537 171.268 7.46
0.018
Interaction 1 0.438 0.438 0.438
0.894 0.02

Residual 7 160.610 160.610 22.944


Error
Lack-of-Fit 3 105.405 105.405 35.135 2.55
0.194
Pure Error 4 55.206 55.206 13.801
Total 12 508.548

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Obs StdOrder Yield Fit SE Fit Residual St Resid

1 5 34.788 28.993 3.787 5.795 1.98

2 12 35.397 39.028 2.142 -3.632 -0.85

3 2 30.627 27.417 3.787 3.210 1.09

4 8 31.075 29.073 3.787 2.002 0.68

5 10 37.824 39.028 2.142 -1.204 -0.28

6 3 23.805 28.923 3.787 -5.118 -1.74

7 6 22.880 26.768 3.787 -3.887 -1.33

8 9 44.909 39.028 2.142 5.881 1.37

9 7 29.075 29.169 3.787 -0.094 -0.03

10 4 29.739 28.011 3.787 1.728 0.59

11 11 36.856 39.028 2.142 -2.172 -0.51

12 1 26.017 29.653 3.787 -3.636 -1.24

13 13 40.155 39.028 2.142 1.127 0.26

As a criterion, p-values should be below 0.05 in order to attest the correctness of


the experiment. Since, p-values for time and temp*time is beyond the criterion, one of
the term which is temp*time was deleted. After deleting the temp*time (Tt) term, surface
analysis was done again. The results showed that outliers existed in the data of standard
order 5 and 9. Then, this standard values were deleted to remove the residual values.
Finally, after deleting temp*time (Tt) and standard order 5 and 9, an output of
coded units were illustrated in Table 4.3 below.

Table 4.3. Final Response Surface Regression: Yield versus temp, time

Estimated Regression Coefficients for Yield


Term Coef SE Coef T P
Constant -502.276 72.6670 -6.912 0.000
temp 1.676 0.2370 7.072 0.000
time 0.487 0.1343 3.626 0.011
temp*temp -0.001 0.0002 -7.126 0.000
time*time -0.002 0.0006 -3.670 0.010

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S = 2.17112 PRESS = 125.035
R-Sq = 91.47% R-Sq(pred) = 62.27% R-Sq(adj) = 85.78%

Analysis of Variance for Yield


Source DF Seq SS Adj SS Adj MS F P
Regression 4 303.141 303.141 75.785 16.08 0.002
Linear 2 0.279 299.875 149.938 31.81 0.001
Square 2 302.862 302.862 151.431 32.13 0.001
Residual Error 6 28.283 28.283 4.714

Lack-of-Fit 3 16.305 16.305 5.435 1.36 0.403


Pure Error 3 11.978 11.978 3.993
Total 10 331.423

Obs StdOrder Yield Fit SE Fit Residual St Resid


1 12 35.397 37.558 1.086 -2.161 -1.15

2 2 30.627 28.548 1.342 2.079 1.22

3 8 31.075 31.005 1.773 0.070 0.06


4 10 37.824 37.558 1.086 0.266 0.14

5 3 23.805 24.591 1.707 -0.786 -0.59

6 6 22.880 24.836 1.773 -1.956 -1.56


7 7 29.075 31.101 1.773 -2.026 -1.62

8 4 29.739 28.480 1.342 1.259 0.74

9 11 36.856 37.558 1.086 -0.702 -0.37


10 1 26.017 24.659 1.707 1.358 1.01

11 13 40.155 37.558 1.086 2.597 1.38

Term Coef

Constant -502.276

temp 1.67628
time 0.487049

temp*temp -0.00137529

time*time -0.00203291

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From the estimated regression coefficients for yield, the data suggested a
correlation of:

𝑌 = −502.276 + 1.6763𝑇 + 0.487𝑡 − 0.00138𝑇 2 − 0.00204𝑡 2

Figure 4.1 below illustrates the optimum yield obtained. The surface plot was
constructed using Minitab ® 15 and it shows that the optimum temperature is 607.36°C
with carbonization time of 119.36 minutes. The minimum points within the curve are
706°C and 494°C with both 120 minutes of carbonization time. The behavior of the
minimum and maximum temperatures set shows that the yield is high for 494°C and low
yield for 706°C due to burning. The optimum temperature and time can be solved
mathematically.

Figure 4.1. Surface plot of Y vs. Time, Temp

After obtaining the optimum time and temperature, the values were substituted to
the equation:

𝑌 = −502.276 + 1.6763𝑇 + 0.487𝑡 − 0.00138𝑇 2 − 0.00204𝑡 2


where: T - temperature in oC
t - time in minutes

Using the optimum values, the Yopt attained is 35.84%.

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4.2 Determination of Adsorption Capacity

Adsorption capacity is the amount of solute from aqueous solution that is


adsorbed per mass of adsorbent. From the experiment, the AC that has the lowest
adsorption was from the temperature 494.934oC carbonized for 120 minutes. The AC
produced from 706oC for 120 minutes had the highest adsorption of MB. Table 4.4
shows the data of adsorption capacities based on the experiments.

Table 4.4. Data of Adsorption Capacity


Time,
StdOrder RunOrder Blocks Temp, C min %Yield Q (mg/g)
4 1 1 675 160 29.74 123.59
5 2 1 494 120 34.79 59.33
3 3 1 525 160 23.80 86.40
1 4 1 525 80 26.02 61.52
9 5 1 600 120 35.40 104.27
10 6 1 600 120 37.82 93.76
8 7 1 600 177 31.07 113.36
12 8 1 600 120 44.91 98.81
2 9 1 675 80 30.63 118.33
13 10 1 600 120 36.86 101.17
7 11 1 600 63 29.07 63.90
11 12 1 600 120 40.15 103.46
6 13 1 706 120 22.88 124.72

Table 4.5 below shows the initial Minitab ® 15 response surface regression of
Adsorption Capacity (Q) against temperature and time. The analysis was done using
uncoded units. Meaning, the estimated regression as well as the full table will only be
presented.

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Table 4.5. Initial Response Surface Regression: Adsorption Capacity versus temp,
time

Estimated Regression Coefficients for Q


Term Coef SE Coef T P
Constant -428.401 200.964 -2.132 0.070
Temp, C 1.009 0.608 1.659 0.141
Time, min 1.902 0.841 2.262 0.058
Temp, C*Temp, C -0.000 0.000 -0.851 0.423
Time, min*Time, min -0.003 0.002 -1.467 0.186
Temp, C*Time, min -0.002 0.001 -1.347 0.220

S = 7.28604 PRESS = 2245.48


R-Sq = 94.01% R-Sq(pred) = 63.81% R-Sq(adj) = 89.73%

Analysis of Variance for Q


Source DF Seq SS Adj SS Adj MS F P
Regression 5 5832.78 5832.78 1166.56 21.97 0.000
Linear 2 5598.78 334.55 167.27 3.15 0.106
Temp, C 1 4346.51 146.08 146.08 2.75 0.141
Time, min 1 1252.28 271.66 271.66 5.12 0.058
Square 2 137.74 137.74 68.87 1.30 0.332
Temp, C*Temp, C 1 23.52 38.46 38.46 0.72 0.423
Time, min*Time, min 1 114.23 114.23 114.23 2.15 0.186
Interaction 1 96.25 96.25 96.25 1.81 0.220
Temp, C*Time, min 1 96.25 96.25 96.25 1.81 0.220
Residual Error 7 371.60 371.60 53.09
Lack-of-Fit 3 300.05 300.05 100.02 5.59 0.065
Pure Error 4 71.56 71.56 17.89
Total 12 6204.38

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Obs StdOrder Q Fit SE Fit Residual St Resid
1 4 123.586 124.807 5.760 -1.221 -0.27
2 5 59.330 62.629 5.760 -3.299 -0.74
3 3 86.401 88.000 5.760 -1.599 -0.36
4 1 61.518 53.166 5.760 8.352 1.87
5 9 104.270 100.295 3.258 3.975 0.61
6 10 93.756 100.295 3.258 -6.539 -1.00
7 8 113.356 109.885 5.760 3.471 0.78
8 12 98.815 100.295 3.258 -1.480 -0.23
9 2 118.325 109.595 5.760 8.730 1.96
10 13 101.172 100.295 3.258 0.877 0.13
11 7 63.895 74.497 5.760 -10.602 -2.38 R
12 11 103.464 100.295 3.258 3.168 0.49
13 6 124.724 128.557 5.760 -3.833 -0.86

The p-values in the table are beyond 0.05 and standard order 7 is considered an
outlier. Standard order 7 was deleted and surface analysis was done again. The result
showed that standard order 10 and 12 existed as an outlier and time*time (t2) has a p-
value greater than 0.05. After removing standard order 10 and 12, and time*time (t2), an
output of coded units were illustrated in Table 4.6.

Table 4.6. Final Response Surface Regression: Adsorption Capacity versus temp,
time

Estimated Regression Coefficients for Q


Term Coef SE Coef T P
Constant 102.915 0.5035 204.405 0.000
Temp, C 23.309 0.3706 62.903 0.000
Time, min 7.485 0.4440 16.857 0.000
Temp, C*Temp, C -5.448 0.4519 -12.057 0.000
Temp, C*Time, min -4.905 0.5240 -9.361 0.000

S = 1.04809 PRESS = 11.1556


R-Sq = 99.89% R-Sq(pred) = 99.78% R-Sq(adj) = 99.80%

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Analysis of Variance for Q
Source DF Seq SS Adj SS Adj MS F P
Regression 4 5026.20 5026.20 1256.55 1143.90 0.000
Linear 2 4770.26 4658.63 2329.32 2120.49 0.000
Temp, C 1 4346.51 4346.51 4346.51 3956.83 0.000
Time, min 1 423.76 312.13 312.13 284.15 0.000
Square 1 159.68 159.68 159.68 145.36 0.000
Temp, C*Temp, C 1 159.68 159.68 159.68 145.36 0.000
Interaction 1 96.25 96.25 96.25 87.62 0.000
Temp, C*Time, min 1 96.25 96.25 96.25 87.62 0.000

Residual Error 5 5.49 5.49 1.10


Lack-of-Fit 3 0.33 0.33 0.11 0.04 0.986
Pure Error 2 5.17 5.17 2.58
Total 9 5031.69

Obs StdOrder Q Fit SE Fit Residual St Resid


1 4 123.586 123.355 0.830 0.231 0.36
2 5 59.330 59.054 0.818 0.276 0.42
3 3 86.401 86.548 0.830 -0.147 -0.23
4 1 61.518 61.767 0.877 -0.249 -0.43
5 9 104.270 102.915 0.503 1.355 1.47

6 8 113.356 113.500 0.692 -0.144 -0.18


7 2 118.325 118.196 0.877 0.129 0.22
8 13 101.172 102.915 0.503 -1.743 -1.90
9 11 103.464 102.915 0.503 0.549 0.60
10 6 124.724 124.982 0.818 -0.258 -0.39

Term Coef
Constant -572.433
Temp, C 1.66931
Time, min 1.16821
Temp, C*Temp, C -9.68584E-04
Temp, C*Time, min -0.00163514

Figure 4.2 illustrates the surface plot constructed using Minitab ® 15 for the
adsorption capacity (Q) versus time and temperature. As observed from the graph, the
adsorption capacity of an AC increases with increased carbonization temperature and

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time. Use of higher temperature and enough time for carbonization would have larger
possibility of removing impurities and effectively derive the Breadnut peel into AC.

Figure 4.2. Surface plot of Q vs. Time, Temp

The optimum temperature and time estimated that can produce AC with highest
adsorption is at 712.317oC for 176.46 minutes. The Qopt was computed from the
generated equation

𝑄 = −572.433 + 1.6693𝑇 + 1.1682𝑡 − 9.686 × 10−4 𝑇 4 − 0.00164𝑇𝑡


where: T - temperature in oC
t - time in minutes

The Qopt that was estimated is 125.174 milligram of MB per gram of activated carbon.

4.3 Determination on the Amount of Removed Pollutant per Weight of Dried


Material, Y*Q

For the estimation of the amount of pollutant that can be removed per weight of
dried material, the yield (Y) and adsorption capacity (Q) was plotted with its temperature
and time. Table 4.7. shows the data of the amount of removed pollutant per weight of
dried material.

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Table 4.7. Data of amount of removed pollutant per weight of
dried material (Y*Q)
Time,
StdOrder RunOrder Blocks Temp, C %Yield Q (mg/g) Y*Q
min
4 1 1 675 160 29.74 123.59 36.75
5 2 1 494 120 34.79 59.33 20.64
3 3 1 525 160 23.80 86.40 20.57
1 4 1 525 80 26.02 61.52 16.01
9 5 1 600 120 35.40 104.27 36.91
10 6 1 600 120 37.82 93.76 35.46
8 7 1 600 177 31.07 113.36 35.22
12 8 1 600 120 44.91 98.81 44.38
2 9 1 675 80 30.63 118.33 36.24
13 10 1 600 120 36.86 101.17 37.29
7 11 1 600 63 29.07 63.90 18.58
11 12 1 600 120 40.15 103.46 41.55
6 13 1 706 120 22.88 124.72 28.54

Table 4.8 below shows the initial Minitab ® 15 response surface regression of the
amount of removed pollutant per weight of dried sample against temperature and time.
The analysis was done using uncoded units. Meaning, the estimated regression as well
as the full table will only be presented.

Table 4.8. Initial Response Surface Regression: Y*Q versus temp, time

Estimated Regression Coefficients for Y*Q


Term Coef SE Coef T P
Constant -533.298 140.986 -3.783 0.007
Temp, C 1.582 0.427 3.708 0.008
Time, min 1.146 0.590 1.944 0.093
Temp, C*Temp, C -0.001 0.000 -3.536 0.010
Time, min*Time, min -0.004 0.001 -2.939 0.022
Temp, C*Time, min -0.000 0.001 -0.396 0.704

S = 5.11150 PRESS = 994.624


R-Sq = 82.78% R-Sq(pred) = 6.37% R-Sq(adj) = 70.49%

20
Analysis of Variance for Y*Q
Source DF Seq SS Adj SS Adj MS F P
Regression 5 879.39 879.394 175.879 6.73 0.013
Linear 2 385.48 384.202 192.101 7.35 0.019
Temp, C 1 283.10 359.173 359.173 13.75 0.008
Time, min 1 102.38 98.694 98.694 3.78 0.093
Square 2 489.82 489.816 244.908 9.37 0.010
Temp, C*Temp, C 1 264.13 326.623 326.623 12.50 0.010
Time, min*Time,min 1 225.69 225.687 225.687 8.64 0.022
Interaction 1 4.10 4.098 4.098 0.16 0.704
Temp, C*Time, min 1 4.10 4.098 4.098 0.16 0.704
Residual Error 7 182.89 182.892 26.127
Lack-of-Fit 3 127.75 127.753 42.584 3.09 0.152
Pure Error 4 55.14 55.139 13.785
Total 12 1062.29

Obs StdOrder Y*Q Fit SE Fit Residual St Resid


1 4 36.754 35.082 4.041 1.671 0.53
2 5 20.640 16.999 4.041 3.640 1.16
3 3 20.568 25.209 4.041 -4.641 -1.48
4 1 16.005 16.030 4.041 -0.025 -0.01
5 9 36.908 39.116 2.286 -2.208 -0.48
6 10 35.463 39.116 2.286 -3.654 -0.80
7 8 35.225 32.784 4.041 2.441 0.78
8 12 44.377 39.116 2.286 5.260 1.15
9 2 36.240 29.952 4.041 6.288 2.01 R
10 13 37.288 39.116 2.286 -1.828 -0.40
11 7 18.577 22.665 4.041 -4.088 -1.31
12 11 41.545 39.116 2.286 2.429 0.53
13 6 28.537 33.825 4.041 -5.287 -1.69

The p-values for time and temp*time is beyond the criterion and standard
order 2 is considered an outlier. Standard order 2 and temp*time (Tt) were removed.
Table 4.9 shows the coded units of the surface analysis.

21
Table 4.9. Final Response Surface Regression: Y*Q versus temp, time

Estimated Regression Coefficients for Y*Q


Term Coef SE Coef T P
Constant 39.116 1.705 22.945 0.000
Temp, C 4.489 1.476 3.040 0.019
Time, min 5.037 1.476 3.412 0.011
Temp, C*Temp, C -7.582 1.476 -5.136 0.001
Time, min*Time, min -6.426 1.476 -4.352 0.003

S = 3.81203 PRESS = 327.774


R-Sq = 90.19% R-Sq(pred) = 68.39% R-Sq(adj) = 84.58%

Analysis of Variance for Y*Q


Source DF Seq SS Adj SS Adj MS F P
Regression 4 935.13 935.13 233.78 16.09 0.001
Linear 2 369.14 363.85 181.92 12.52 0.005
Temp, C 1 259.19 134.32 134.32 9.24 0.019
Time, min 1 109.95 169.17 169.17 11.64 0.011
Square 2 565.99 565.99 283.00 19.47 0.001
Temp, C*Temp, C 1 290.71 383.26 383.26 26.37 0.001
Time, min*Time, min 1 275.28 275.28 275.28 18.94 0.003
Residual Error 7 101.72 101.72 14.53
Lack-of-Fit 3 46.58 46.58 15.53 1.13 0.438
Pure Error 4 55.14 55.14 13.78
Total 11 1036.85

Obs StdOrder Y*Q Fit SE Fit Residual St Resid


1 4 36.754 34.634 2.411 2.119 0.72
2 5 20.640 17.604 3.024 3.036 1.31
3 3 20.568 25.657 2.411 -5.089 -1.72
4 1 16.005 15.582 2.411 0.423 0.14
5 9 36.908 39.116 1.705 -2.208 -0.65
6 10 35.463 39.116 1.705 -3.654 -1.07
7 8 35.225 33.389 3.024 1.836 0.79
8 12 44.377 39.116 1.705 5.260 1.54
9 13 37.288 39.116 1.705 -1.828 -0.54
10 7 18.577 19.140 3.347 -0.563 -0.31
11 11 41.545 39.116 1.705 2.429 0.71
12 6 28.537 30.300 3.347 -1.762 -0.97

22
Term Coef
Constant -554.997
Temp, C 1.67738
Time, min 1.08982
Temp, C*Temp, C -0.00134794
Time, min*Time, min -0.00401616

Figure 4.3 illustrates the surface plot of Y*Q versus temperature and time.

Figure 4.3. Surface plot of Y*Q vs. Time, Temp

The generated equation for the plot is

𝑌 ∗ 𝑄 = −544.997 + 1.6774𝑇 − 1.0898𝑡 − 0.00135𝑇 2 − 0.00402𝑡 2

where: Y*Q – the amount of pollutant removed per weight of dried material
T- Temperature in oC
t – time in minutes

23
The obtained optimum temperature and time from the equation are 621.26°C and
135.55 minutes, respectively. Using these optimum parameters in the equation, the
estimated amount of pollutant removed per weight of dried raw material is 39.913
milligram of MB per gram of dried material.

Economically, this means that the effectiveness of the product obtained from the
activated carbon would be maximized as well as the yield.

24
CHAPTER 5

Conclusion and Recommendations

Based on the analyses drawn together, the research proved that breadnut peels
can be an alternative raw material for preparation of activated carbon.

The estimated optimum yield is 35.84% at the optimum conditions of 607.36 oC


for 119.36 minutes. Correlation for the %yield is given by:

𝑌 = −502.276 + 1.6763𝑇 + 0.487𝑡 − 0.00138𝑇 2 − 0.00204𝑡 2

The produced AC that can have the highest adsorption capacity can be derived
with the optimum temperature and time estimated which is at 712.317oC for 176.46
minutes. The study also showed that as temperature increases, the adsorption capacity
increases. Thus, they are directly proportional to each other. The correlation for the
adsorption capacity is given:

𝑄 = −572.433 + 1.6693𝑇 + 1.1682𝑡 − 9.686 × 10−4 𝑇 4 − 0.00164𝑇𝑡

Since the obtained estimated optimum time and temperature for adsorption
capacity is beyond the parameter conditions that were set in the experiment, it is
recommended to further refine the study by setting the conditions near the estimated
values to justify the correlation.

In terms of amount of removed pollutant per weight of dried material, the


optimum parameters are 621.26°C and 135.55 minutes. Using the computed
parameters, the optimum amount of pollutant removed per weight of dried raw material
is 39.913 milligram of MB of dried raw material derived from the equation:

𝑌 ∗ 𝑄 = −544.997 + 1.6774𝑇 − 1.0898𝑡 − 0.00135𝑇 2 − 0.00402𝑡 2

25
These results shows that in choosing the appropriate correlation, factors such as
the desired yield, adsorption capacity and the amount of pollutant removed per weight of
dried raw material should be considered.

It is recommended to sieve the activated carbon derived from breadnut


(Artocarpus camansi) to obtain the uniform particle size of the product. Comparison with
the commercially available activated carbon can be done using the available data to
assess the efficacy of the produced activated carbon with respect to yield (Y), adsorptive
capacity (Q) and amount of removed pollutant per dried raw material (Y*Q).

It is suggested to study the effects of concentration on the adsorption isotherm of


the activated carbon derived from breadnut peel. It is also suggested to conduct further
tests on metals and industrial effluent as well as considering factors such as cost and
equipment.

26
Bibliography

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1901/index.

El Mouzdahir, Y., A. Elmchaouri, R. Mahboub, A. Gil and S. A. Korili (2010). "Equilibrium


modeling for the adsorption of methylene blue from aqueous solutions on
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Operations, John Wiley and Sons (Asia) PTE LTD.

Garg, V. K., M. Amita, R. Kumar and R. Gupta (2004). "Basic dye (methylene blue)
removal from simulated wastewater by adsorption using Indian Rosewood
sawdust: a timber industry waste." Dyes and Pigments 63(3): 243-250.

Geankoplis, C. J. (2003). Principles of Transport Processes and Separation Processes,


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Kadirvelu, K., K. Thamaraiselvi and C. Namasivayam (2001). "Adsorption of nickel(II)


from aqueous solution onto activated carbon prepared from coirpith." Separation
and Purification Technology 24(3): 497-505.

Kavitha, D. and C. Namasivayam (2007). "Experimental and kinetic studies on


methylene blue adsorption by coir pith carbon." Bioresource Technology 98(1):
14-21.

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Khaled, A., El Nemr, A., El-Sikaily, A., Abdelwahab, O. (2009). "Treatment of Artificial
Textile Dye Effluent Containing Direct Yellow 12 by Orange Peel Carbon."
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dehydrated wheat bran carbon." Journal of Hazardous Materials 146(1–2):
262-269.

Prahas, D., Y. Kartika, N. Indraswati and S. Ismadji (2008). "The Use of Activated
Carbon Prepared from Jackfruit (Artocarpus heterophyllus) Peel for Methylene
Blue Removal." Journal of Environmental Protection Science 2: 1-10.

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blue on low-cost adsorbents: A review." Journal of Hazardous Materials
177(1–3): 70-80.

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Company.

Weng, C.-H., C.-Z. Tsai, S.-H. Chu and Y. C. Sharma (2007). "Adsorption characteristics
of copper(II) onto spent activated clay." Separation and Purification Technology
54(2): 187-197.

Yin, C. Y., M. K. Aroua and W. M. A. W. Daud (2007). "Review of modifications of


activated carbon for enhancing contaminant uptakes from aqueous solutions."
Separation and Purification Technology 52(3): 403-415.

28
Zhang, Z., Z. Zhang, Y. Fernandez, J. A. Menendez, H. Niu, J. Peng, L. Zhang and S.
Guo (2009). "Adsorption isotherms and kinetics of methylene blue on a low-cost
adsorbent recovered from a spent catalyst of vinyl acetate synthesis." Applied
Surface Science 256(8): 2569-2576.

29
APPENDIX A

Preliminary Calculation, Calibration Data and


Adsorption Capacity

30
APPENDIX A

Preliminary Calculation, Calibration Data and Adsorption Capacity

A.1 Preparation of Methylene Blue Solution

500 𝑚𝑔 𝑀𝑒𝑡ℎ𝑦𝑙𝑒𝑛𝑒 𝐵𝑙𝑢𝑒


250 𝑝𝑝𝑚 𝑀𝐵 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 =
2 𝐿𝑖𝑡𝑒𝑟𝑠 𝑜𝑓 𝑑𝑖𝑠𝑡𝑖𝑙𝑙𝑒𝑑 𝑤𝑎𝑡𝑒𝑟

A.2 Calculation for Dilution

𝐶1 𝑉1 = 𝐶2 𝑉2

Where:
C1 =Initial concentration MB Solution
V1 = Volume of initial concentration MB solution
C2 = Final concentration of diluted MB solution
V2 = Volume of diluted MB solution

Sample Calculation (Diluting 250 ppm to 20 mL of 30 ppm of Methylene Blue solution)

(250 𝑝𝑝𝑚)(𝑉1) = (30 𝑝𝑝𝑚)(20 𝑚𝐿)


V1 = 2.4 mL of 250 ppm of MB solution
Volume of water = 20 – 2.4 = 17.6 mL

31
A.3 Calibration Curve

Table A.3. Calibration Curve


Concentration (ppm) Absorbance

30 1.614

25 1.361

20 1.155

15 0.836

12.5 0.745

10 0.609

7.5 0.463

5 0.256

2.5 0.138

0 0

Calibration Curve
1.5
y = 0.057935x + 0.000216
Absorbance

R² = 0.995804
1

0.5

0
0 5 10 15 20 25
Concentration

Figure A.3. Calibration Curve

32
Sample calculation of concentration of adsorbed solution given the absorbance
Absorbance = 0.022 (Temp = 706; time = 120 mins)
Using linear regression,

𝐴 = 0.057935𝐶 + 0.000216
Where A = absorbance
C = concentration
0.022 − 0.000216
𝐶=
0.057935
C = 0.3760 ppm

A.4 Calculation of Adsorption Capacity

(𝐶𝑜 − 𝐶)𝑉
𝑄=
𝑊

Where:
Q = adsorption capacity
(Amount of solute from aqueous solution that is adsorbed per mass of adsorbent)
Co = initial concentration of MB solution
C = final concentration of MB solution
V = Volume of solution
W = mass of adsorbent

Sample calculation of adsorption capacity


Given: Initial Concentration (Co) = 250 ppm
Final Concentration (C) = 0.3760 ppm
Amount of activated carbon used (W) = 0.1208 g
Volume of Methylene Blue solution (V) = 51.4 mL

(250 − 0.3760)(0.0514)
𝑄=
(0.1208)
Q = 124.8120 mg/g

33
APPENDIX B

Curve Fitting of Percent Yield

34
APPENDIX B

Curve Fitting of Percent Yield

B.1. Data of Percent Yield (%Y)

Table B.1. Data of Percent Yield

wt after
wt before
carbonization,
Std Run Temp, Time, activation and %
washing & drying,
Order Order °C min carbonization, g Yield
g
4 1 675 160 5.3821 1.6006 29.74
5 2 494 120 5.844 2.0330 34.79
3 3 525 160 5.9517 1.4168 23.80
1 4 525 80 5.9492 1.5478 26.02
9 5 600 120 4.7078 1.6664 35.40
10 6 600 120 4.2552 1.6095 37.82
8 7 600 177 6.6852 2.0774 31.07
12 8 600 120 4.0609 1.8237 44.91
2 9 675 80 5.7968 1.7754 30.63
13 10 600 120 5.9743 2.2019 36.86
7 11 600 63 6.1823 1.7975 29.07
11 12 600 120 5.8068 2.3317 40.15
6 13 706 120 5.6039 1.2822 22.88

B.2. Response Surface Regression: Yield versus temp, time

The analysis was done using uncoded units.

Estimated Regression Coefficients for Yield

Term Coef SE Coef T P


Constant -347.936 132.119 -2.634 0.034
temp 1.165 0.400 2.915 0.022
time 0.676 0.553 1.223 0.261
temp*temp -0.001 0.000 -3.069 0.018
time*time -0.003 0.001 -2.728 0.029
temp*time 0.000 0.001 0.138 0.894

35
S = 4.79003 PRESS = 835.805
R-Sq = 68.42% R-Sq(pred) = 0.00% R-Sq(adj) = 45.86%

Analysis of Variance for Yield

Source DF Seq SS Adj SS Adj MS F P


Regression 5 347.937 347.937 69.587 3.03 0.090
Linear 2 4.962 199.698 99.849 4.35 0.059
Square 2 342.537 342.537 171.268 7.46 0.018
Interaction 1 0.438 0.438 0.438 0.02 0.894
Residual Error 7 160.610 160.610 22.944
Lack-of-Fit 3 105.405 105.405 35.135 2.55 0.194
Pure Error 4 55.206 55.206 13.801
Total 12 508.548

Obs StdOrder Yield Fit SE Fit Residual St Resid


1 5 34.788 28.993 3.787 5.795 1.98
2 12 35.397 39.028 2.142 -3.632 -0.85
3 2 30.627 27.417 3.787 3.210 1.09
4 8 31.075 29.073 3.787 2.002 0.68
5 10 37.824 39.028 2.142 -1.204 -0.28
6 3 23.805 28.923 3.787 -5.118 -1.74
7 6 22.880 26.768 3.787 -3.887 -1.33
8 9 44.909 39.028 2.142 5.881 1.37
9 7 29.075 29.169 3.787 -0.094 -0.03
10 4 29.739 28.011 3.787 1.728 0.59
11 11 36.856 39.028 2.142 -2.172 -0.51
12 1 26.017 29.653 3.787 -3.636 -1.24
13 13 40.155 39.028 2.142 1.127 0.26

Remove Temp*time

Response Surface Regression: Yield versus temp, time

The analysis was done using uncoded units.

Estimated Regression Coefficients for Yield

Term Coef SE Coef T P


Constant -355.880 111.428 -3.194 0.013
temp 1.179 0.364 3.242 0.012
time 0.742 0.258 2.874 0.021
temp*temp -0.001 0.000 -3.277 0.011
time*time -0.003 0.001 -2.912 0.020

S = 4.48677 PRESS = 597.072


R-Sq = 68.33% R-Sq(pred) = 0.00% R-Sq(adj) = 52.50%

36
Analysis of Variance for Yield

Source DF Seq SS Adj SS Adj MS F P


Regression 4 347.499 347.499 86.875 4.32 0.038
Linear 2 4.962 335.168 167.584 8.32 0.011
Square 2 342.537 342.537 171.268 8.51 0.010
Residual Error 8 161.049 161.049 20.131
Lack-of-Fit 4 105.843 105.843 26.461 1.92 0.272
Pure Error 4 55.206 55.206 13.801
Total 12 508.548

Obs StdOrder Yield Fit SE Fit Residual St Resid


1 5 34.788 28.993 3.547 5.795 2.11 R
2 12 35.397 39.028 2.007 -3.632 -0.90
3 2 30.627 27.748 2.748 2.879 0.81
4 8 31.075 29.073 3.547 2.002 0.73
5 10 37.824 39.028 2.007 -1.204 -0.30
6 3 23.805 29.254 2.748 -5.449 -1.54
7 6 22.880 26.768 3.547 -3.887 -1.41
8 9 44.909 39.028 2.007 5.881 1.47
9 7 29.075 29.169 3.547 -0.094 -0.03
10 4 29.739 27.680 2.748 2.059 0.58
11 11 36.856 39.028 2.007 -2.172 -0.54
12 1 26.017 29.322 2.748 -3.305 -0.93
13 13 40.155 39.028 2.007 1.127 0.28

R denotes an observation with a large standardized residual.

Remove Standard Order 5.

Response Surface Regression: Yield versus temp, time

The analysis was done using uncoded units.

Estimated Regression Coefficients for Yield

Term Coef SE Coef T P


Constant -554.467 103.924 -5.335 0.001
temp 1.833 0.340 5.384 0.001
time 0.597 0.190 3.138 0.016
temp*temp -0.002 0.000 -5.438 0.001
time*time -0.002 0.001 -3.178 0.016

S = 3.19621 PRESS = 189.999


R-Sq = 85.79% R-Sq(pred) = 62.24% R-Sq(adj) = 77.66%

Analysis of Variance for Yield

Source DF Seq SS Adj SS Adj MS F P


Regression 4 431.611 431.611 107.903 10.56 0.004
Linear 2 1.417 423.863 211.932 20.75 0.001
Square 2 430.194 430.194 215.097 21.06 0.001
Residual Error 7 71.510 71.510 10.216
Lack-of-Fit 3 16.305 16.305 5.435 0.39 0.765
Pure Error 4 55.206 55.206 13.801
Total 11 503.121

37
Obs StdOrder Yield Fit SE Fit Residual St Resid
1 12 35.397 39.028 1.429 -3.632 -1.27
2 2 30.627 28.548 1.976 2.079 0.83
3 8 31.075 31.005 2.610 0.070 0.04
4 10 37.824 39.028 1.429 -1.204 -0.42
5 3 23.805 24.591 2.512 -0.786 -0.40
6 6 22.880 24.836 2.610 -1.956 -1.06
7 9 44.909 39.028 1.429 5.881 2.06 R
8 7 29.075 31.101 2.610 -2.026 -1.10
9 4 29.739 28.480 1.976 1.259 0.50
10 11 36.856 39.028 1.429 -2.172 -0.76
11 1 26.017 24.659 2.512 1.358 0.69
12 13 40.155 39.028 1.429 1.127 0.39

R denotes an observation with a large standardized residual.

Remove Standard Order 9.

Response Surface Regression: Yield versus temp, time

The analysis was done using uncoded units.

Estimated Regression Coefficients for Yield

Term Coef SE Coef T P


Constant -502.276 72.6670 -6.912 0.000
temp 1.676 0.2370 7.072 0.000
time 0.487 0.1343 3.626 0.011
temp*temp -0.001 0.0002 -7.126 0.000
time*time -0.002 0.0006 -3.670 0.010

S = 2.17112 PRESS = 125.035


R-Sq = 91.47% R-Sq(pred) = 62.27% R-Sq(adj) = 85.78%

Analysis of Variance for Yield

Source DF Seq SS Adj SS Adj MS F P


Regression 4 303.141 303.141 75.785 16.08 0.002
Linear 2 0.279 299.875 149.938 31.81 0.001
Square 2 302.862 302.862 151.431 32.13 0.001
Residual Error 6 28.283 28.283 4.714
Lack-of-Fit 3 16.305 16.305 5.435 1.36 0.403
Pure Error 3 11.978 11.978 3.993
Total 10 331.423

38
Obs StdOrder Yield Fit SE Fit Residual St Resid
1 12 35.397 37.558 1.086 -2.161 -1.15
2 2 30.627 28.548 1.342 2.079 1.22
3 8 31.075 31.005 1.773 0.070 0.06
4 10 37.824 37.558 1.086 0.266 0.14
5 3 23.805 24.591 1.707 -0.786 -0.59
6 6 22.880 24.836 1.773 -1.956 -1.56
7 7 29.075 31.101 1.773 -2.026 -1.62
8 4 29.739 28.480 1.342 1.259 0.74
9 11 36.856 37.558 1.086 -0.702 -0.37
10 1 26.017 24.659 1.707 1.358 1.01
11 13 40.155 37.558 1.086 2.597 1.38

Estimated Regression Coefficients for Yield using data in uncoded units

Term Coef
Constant -502.276
temp 1.67628
time 0.487049
temp*temp -0.00137529
time*time -0.00203291

B.2. Calculation of Optimum Temperature, Time and %Yield


%𝑌 = 502.276 + 1.6763𝑇 + 0.487𝑡 − 0.00138𝑇 2 − 0.00204𝑡 2
𝑑𝑌
= 0 = 1.6763 − 2(0.00138)𝑇
𝑑𝑇
𝑑𝑌
= 0 = 0.487 − 2(0.00204)𝑡
𝑑𝑡
Topt = 607.36 °C
topt = 119.36 mins
%Yopt = 35.84%

39
APPENDIX C

Curve Fitting of Adsorption Capacity (Q)

40
APPENDIX C

Curve Fitting of Adsorption Capacity (Q)

C.1. Adsorption Capacity (Q) and Optimization as a Function of Time and


Temperature

Table C.1. Data of Adsorption Capacity (Q)


StdOrder RunOrder Blocks Temp, C Time, min %Yield Q (mg/g)
4 1 1 675 160 29.74 123.59
5 2 1 494 120 34.79 59.33
3 3 1 525 160 23.80 86.40
1 4 1 525 80 26.02 61.52
9 5 1 600 120 35.40 104.27
10 6 1 600 120 37.82 93.76
8 7 1 600 177 31.07 113.36
12 8 1 600 120 44.91 98.81
2 9 1 675 80 30.63 118.33
13 10 1 600 120 36.86 101.17
7 11 1 600 63 29.07 63.90
11 12 1 600 120 40.15 103.46
6 13 1 706 120 22.88 124.72

C.2. Response Surface Regression: Q versus Temp, C, Time, min


The analysis was done using uncoded units.

Estimated Regression Coefficients for Q

Term Coef SE Coef T P


Constant -428.401 200.964 -2.132 0.070
Temp, C 1.009 0.608 1.659 0.141
Time, min 1.902 0.841 2.262 0.058
Temp, C*Temp, C -0.000 0.000 -0.851 0.423
Time, min*Time, min -0.003 0.002 -1.467 0.186
Temp, C*Time, min -0.002 0.001 -1.347 0.220

S = 7.28604 PRESS = 2245.48


R-Sq = 94.01% R-Sq(pred) = 63.81% R-Sq(adj) = 89.73%

41
Analysis of Variance for Q

Source DF Seq SS Adj SS Adj MS F P


Regression 5 5832.78 5832.78 1166.56 21.97 0.000
Linear 2 5598.78 334.55 167.27 3.15 0.106
Temp, C 1 4346.51 146.08 146.08 2.75 0.141
Time, min 1 1252.28 271.66 271.66 5.12 0.058
Square 2 137.74 137.74 68.87 1.30 0.332
Temp, C*Temp, C 1 23.52 38.46 38.46 0.72 0.423
Time, min*Time, min 1 114.23 114.23 114.23 2.15 0.186
Interaction 1 96.25 96.25 96.25 1.81 0.220
Temp, C*Time, min 1 96.25 96.25 96.25 1.81 0.220
Residual Error 7 371.60 371.60 53.09
Lack-of-Fit 3 300.05 300.05 100.02 5.59 0.065
Pure Error 4 71.56 71.56 17.89
Total 12 6204.38

Obs StdOrder Q Fit SE Fit Residual St Resid


1 4 123.586 124.807 5.760 -1.221 -0.27
2 5 59.330 62.629 5.760 -3.299 -0.74
3 3 86.401 88.000 5.760 -1.599 -0.36
4 1 61.518 53.166 5.760 8.352 1.87
5 9 104.270 100.295 3.258 3.975 0.61
6 10 93.756 100.295 3.258 -6.539 -1.00
7 8 113.356 109.885 5.760 3.471 0.78
8 12 98.815 100.295 3.258 -1.480 -0.23
9 2 118.325 109.595 5.760 8.730 1.96
10 13 101.172 100.295 3.258 0.877 0.13
11 7 63.895 74.497 5.760 -10.602 -2.38 R
12 11 103.464 100.295 3.258 3.168 0.49
13 6 124.724 128.557 5.760 -3.833 -0.86

R denotes an observation with a large standardized residual.

Remove Standard Order 7.

Response Surface Regression: Q versus Temp, C, Time, min


The analysis was done using uncoded units.

Estimated Regression Coefficients for Q

Term Coef SE Coef T P


Constant -478.787 95.9799 -4.988 0.002
Temp, C 1.386 0.2985 4.642 0.004
Time, min 0.982 0.4396 2.233 0.067
Temp, C*Temp, C -0.001 0.0002 -3.031 0.023
Time, min*Time, min 0.001 0.0011 0.741 0.487
Temp, C*Time, min -0.002 0.0006 -2.835 0.030

S = 3.46059 PRESS = 117.812


R-Sq = 98.58% R-Sq(pred) = 97.67% R-Sq(adj) = 97.40%

42
Analysis of Variance for Q

Source DF Seq SS Adj SS Adj MS F P


Regression 5 4991.10 4991.10 998.220 83.35 0.000
Linear 2 4781.29 290.15 145.073 12.11 0.008
Temp, C 1 4346.51 258.10 258.102 21.55 0.004
Time, min 1 434.78 59.71 59.708 4.99 0.067
Square 2 113.56 113.56 56.780 4.74 0.058
Temp, C*Temp, C 1 106.99 110.02 110.020 9.19 0.023
Time, min*Time, min 1 6.57 6.57 6.568 0.55 0.487
Interaction 1 96.25 96.25 96.253 8.04 0.030
Temp, C*Time, min 1 96.25 96.25 96.253 8.04 0.030
Residual Error 6 71.85 71.85 11.976
Lack-of-Fit 2 0.30 0.30 0.149 0.01 0.992
Pure Error 4 71.56 71.56 17.889
Total 11 5062.95

Obs StdOrder Q Fit SE Fit Residual St Resid


1 4 123.586 123.343 2.751 0.243 0.12
2 5 59.330 59.095 2.826 0.236 0.12
3 3 86.401 86.536 2.751 -0.135 -0.06
4 1 61.518 61.698 3.224 -0.180 -0.14
5 9 104.270 100.295 1.548 3.975 1.28
6 10 93.756 100.295 1.548 -6.539 -2.11 R
7 8 113.356 113.419 2.826 -0.063 -0.03
8 12 98.815 100.295 1.548 -1.480 -0.48
9 2 118.325 118.127 3.224 0.198 0.16
10 13 101.172 100.295 1.548 0.877 0.28
11 11 103.464 100.295 1.548 3.168 1.02
12 6 124.724 125.023 2.826 -0.299 -0.15

R denotes an observation with a large standardized residual.

Remove Standard Order 10.

Response Surface Regression: Q versus Temp, C, Time, min


The analysis was done using uncoded units.

Estimated Regression Coefficients for Q

Term Coef SE Coef T P


Constant -536.822 55.3470 -9.699 0.000
Temp, C 1.560 0.1717 9.087 0.000
Time, min 1.104 0.2458 4.492 0.006
Temp, C*Temp, C -0.001 0.0001 -6.302 0.001
Time, min*Time, min 0.000 0.0006 0.450 0.672
Temp, C*Time, min -0.002 0.0003 -5.114 0.004

S = 1.91852 PRESS = 38.1932


R-Sq = 99.63% R-Sq(pred) = 99.24% R-Sq(adj) = 99.27%

43
Analysis of Variance for Q

Source DF Seq SS Adj SS Adj MS F P


Regression 5 5013.87 5013.87 1002.77 272.44 0.000
Linear 2 4770.69 338.63 169.31 46.00 0.001
Temp, C 1 4346.51 303.91 303.91 82.57 0.000
Time, min 1 424.19 74.26 74.26 20.18 0.006
Square 2 146.92 146.92 73.46 19.96 0.004
Temp, C*Temp, C 1 146.17 146.17 146.17 39.71 0.001
Time, min*Time, min 1 0.74 0.74 0.74 0.20 0.672
Interaction 1 96.25 96.25 96.25 26.15 0.004
Temp, C*Time, min 1 96.25 96.25 96.25 26.15 0.004
Residual Error 5 18.40 18.40 3.68
Lack-of-Fit 2 0.30 0.30 0.15 0.02 0.976
Pure Error 3 18.11 18.11 6.04
Total 10 5032.27

Obs StdOrder Q Fit SE Fit Residual St Resid


1 4 123.586 123.343 1.525 0.243 0.21
2 5 59.330 59.095 1.566 0.236 0.21
3 3 86.401 86.536 1.525 -0.135 -0.12
4 1 61.518 61.698 1.787 -0.180 -0.26
5 9 104.270 101.930 0.959 2.340 1.41
6 8 113.356 113.419 1.566 -0.063 -0.06
7 12 98.815 101.930 0.959 -3.115 -1.87
8 2 118.325 118.127 1.787 0.198 0.28
9 13 101.172 101.930 0.959 -0.758 -0.46
10 11 103.464 101.930 0.959 1.533 0.92
11 6 124.724 125.023 1.566 -0.299 -0.27

Remove Time*Time

Response Surface Regression: Q versus Temp, C, Time, min


The analysis was done using uncoded units.

Estimated Regression Coefficients for Q

Term Coef SE Coef T P


Constant -540.948 50.8246 -10.643 0.000
Temp, C 1.560 0.1599 9.758 0.000
Time, min 1.173 0.1796 6.529 0.001
Temp, C*Temp, C -0.001 0.0001 -6.768 0.001
Temp, C*Time, min -0.002 0.0003 -5.492 0.002

S = 1.78646 PRESS = 34.1185


R-Sq = 99.62% R-Sq(pred) = 99.32% R-Sq(adj) = 99.37%

44
Analysis of Variance for Q

Source DF Seq SS Adj SS Adj MS F P


Regression 4 5013.12 5013.12 1253.28 392.70 0.000
Linear 2 4770.69 372.27 186.13 58.32 0.000
Temp, C 1 4346.51 303.91 303.91 95.23 0.000
Time, min 1 424.19 136.03 136.03 42.62 0.001
Square 1 146.17 146.17 146.17 45.80 0.001
Temp, C*Temp, C 1 146.17 146.17 146.17 45.80 0.001
Interaction 1 96.25 96.25 96.25 30.16 0.002
Temp, C*Time, min 1 96.25 96.25 96.25 30.16 0.002
Residual Error 6 19.15 19.15 3.19
Lack-of-Fit 3 1.04 1.04 0.35 0.06 0.979
Pure Error 3 18.11 18.11 6.04
Total 10 5032.27

Obs StdOrder Q Fit SE Fit Residual St Resid


1 4 123.586 123.280 1.414 0.306 0.28
2 5 59.330 59.310 1.389 0.020 0.02
3 3 86.401 86.473 1.414 -0.072 -0.07
4 1 61.518 61.330 1.479 0.189 0.19
5 9 104.270 102.146 0.774 2.124 1.32
6 8 113.356 112.987 1.153 0.368 0.27
7 12 98.815 102.146 0.774 -3.331 -2.07 R
8 2 118.325 117.759 1.479 0.566 0.57
9 13 101.172 102.146 0.774 -0.974 -0.60
10 11 103.464 102.146 0.774 1.318 0.82
11 6 124.724 125.238 1.389 -0.514 -0.46

R denotes an observation with a large standardized residual.

Remove Standard Order 12.

Response Surface Regression: Q versus Temp, C, Time, min


The analysis was done using uncoded units.

Estimated Regression Coefficients for Q

Term Coef SE Coef T P


Constant -572.433 31.1264 -18.391 0.000
Temp, C 1.669 0.0988 16.899 0.000
Time, min 1.168 0.1054 11.084 0.000
Temp, C*Temp, C -0.001 0.0001 -12.057 0.000
Temp, C*Time, min -0.002 0.0002 -9.361 0.000

S = 1.04809 PRESS = 11.1556


R-Sq = 99.89% R-Sq(pred) = 99.78% R-Sq(adj) = 99.80%

45
Analysis of Variance for Q

Source DF Seq SS Adj SS Adj MS F P


Regression 4 5026.20 5026.20 1256.55 1143.90 0.000
Linear 2 4770.26 384.18 192.09 174.87 0.000
Temp, C 1 4346.51 313.71 313.71 285.59 0.000
Time, min 1 423.76 134.96 134.96 122.86 0.000
Square 1 159.68 159.68 159.68 145.36 0.000
Temp, C*Temp, C 1 159.68 159.68 159.68 145.36 0.000
Interaction 1 96.25 96.25 96.25 87.62 0.000
Temp, C*Time, min 1 96.25 96.25 96.25 87.62 0.000
Residual Error 5 5.49 5.49 1.10
Lack-of-Fit 3 0.33 0.33 0.11 0.04 0.986
Pure Error 2 5.17 5.17 2.58
Total 9 5031.69

Obs StdOrder Q Fit SE Fit Residual St Resid


1 4 123.586 123.355 0.830 0.231 0.36
2 5 59.330 59.054 0.818 0.276 0.42
3 3 86.401 86.548 0.830 -0.147 -0.23
4 1 61.518 61.767 0.877 -0.249 -0.43
5 9 104.270 102.915 0.503 1.355 1.47
6 8 113.356 113.500 0.692 -0.144 -0.18
7 2 118.325 118.196 0.877 0.129 0.22
8 13 101.172 102.915 0.503 -1.743 -1.90
9 11 103.464 102.915 0.503 0.549 0.60
10 6 124.724 124.982 0.818 -0.258 -0.39

Response Surface Regression: Q versus Temp, C, Time, min


The analysis was done using coded units.

Estimated Regression Coefficients for Q

Term Coef SE Coef T P


Constant 102.915 0.5035 204.405 0.000
Temp, C 23.309 0.3706 62.903 0.000
Time, min 7.485 0.4440 16.857 0.000
Temp, C*Temp, C -5.448 0.4519 -12.057 0.000
Temp, C*Time, min -4.905 0.5240 -9.361 0.000

S = 1.04809 PRESS = 11.1556


R-Sq = 99.89% R-Sq(pred) = 99.78% R-Sq(adj) = 99.80%

Analysis of Variance for Q

Source DF Seq SS Adj SS Adj MS F P


Regression 4 5026.20 5026.20 1256.55 1143.90 0.000
Linear 2 4770.26 4658.63 2329.32 2120.49 0.000
Temp, C 1 4346.51 4346.51 4346.51 3956.83 0.000
Time, min 1 423.76 312.13 312.13 284.15 0.000
Square 1 159.68 159.68 159.68 145.36 0.000
Temp, C*Temp, C 1 159.68 159.68 159.68 145.36 0.000
Interaction 1 96.25 96.25 96.25 87.62 0.000
Temp, C*Time, min 1 96.25 96.25 96.25 87.62 0.000
Residual Error 5 5.49 5.49 1.10
Lack-of-Fit 3 0.33 0.33 0.11 0.04 0.986
Pure Error 2 5.17 5.17 2.58
Total 9 5031.69

46
Obs StdOrder Q Fit SE Fit Residual St Resid
1 4 123.586 123.355 0.830 0.231 0.36
2 5 59.330 59.054 0.818 0.276 0.42
3 3 86.401 86.548 0.830 -0.147 -0.23
4 1 61.518 61.767 0.877 -0.249 -0.43
5 9 104.270 102.915 0.503 1.355 1.47
6 8 113.356 113.500 0.692 -0.144 -0.18
7 2 118.325 118.196 0.877 0.129 0.22
8 13 101.172 102.915 0.503 -1.743 -1.90
9 11 103.464 102.915 0.503 0.549 0.60
10 6 124.724 124.982 0.818 -0.258 -0.39

Estimated Regression Coefficients for Q using data in uncoded units

Term Coef
Constant -572.433
Temp, C 1.66931
Time, min 1.16821
Temp, C*Temp, C -9.68584E-04
Temp, C*Time, min -0.00163514

C.3. Calculation of Optimum Temperature, Time and Adsorption Capacity (Q)


𝑄 = −572.433 + 1.6693𝑇 + 1.1682𝑡 − 9.686 × 10−4 𝑇 2 − 0.00164𝑇𝑡
𝑑𝑄
= 0 = 1.6693 − 2(9.686 × 10−4 )𝑇 − 0.00164𝑡
𝑑𝑇
𝑑𝑄
= 0 = 1.1682 − 0.00164𝑡
𝑑𝑡
topt = 176.46 mins
Topt = 712.32 °C
Qopt =125.174 mg removed pollutant per gram of activated carbon

47
APPENDIX D

Curve Fitting of Amount of Removed


Pollutant per Amount of Dried Material
(Y*Q)

48
APPENDIX D

Curve Fitting of Amount of Removed Pollutant per Amount of Dried Material


(Y*Q)

D.1. Amount of Removed Pollutant per Amount of Dried Material (Y*Q) and
Optimization as a Function of Time and Temperature

Table D.1. Data of Amount of Removed Pollutant per Amount of Dried Material (Y*Q)
Time,
StdOrder RunOrder Blocks Temp, C min %Yield Q (mg/g) Y*Q
4 1 1 675 160 29.74 123.59 36.75
5 2 1 494 120 34.79 59.33 20.64
3 3 1 525 160 23.80 86.40 20.57
1 4 1 525 80 26.02 61.52 16.01
9 5 1 600 120 35.40 104.27 36.91
10 6 1 600 120 37.82 93.76 35.46
8 7 1 600 177 31.07 113.36 35.22
12 8 1 600 120 44.91 98.81 44.38
2 9 1 675 80 30.63 118.33 36.24
13 10 1 600 120 36.86 101.17 37.29
7 11 1 600 63 29.07 63.90 18.58
11 12 1 600 120 40.15 103.46 41.55
6 13 1 706 120 22.88 124.72 28.54

D.2. Central Composite Design: Y*Q versus Temp, C, Time, min


The analysis was done using uncoded units.

Estimated Regression Coefficients for Y*Q

Term Coef SE Coef T P


Constant -533.298 140.986 -3.783 0.007
Temp, C 1.582 0.427 3.708 0.008
Time, min 1.146 0.590 1.944 0.093
Temp, C*Temp, C -0.001 0.000 -3.536 0.010
Time, min*Time, min -0.004 0.001 -2.939 0.022
Temp, C*Time, min -0.000 0.001 -0.396 0.704

S = 5.11150 PRESS = 994.624


R-Sq = 82.78% R-Sq(pred) = 6.37% R-Sq(adj) = 70.49%

49
Analysis of Variance for Y*Q

Source DF Seq SS Adj SS Adj MS F P


Regression 5 879.39 879.394 175.879 6.73 0.013
Linear 2 385.48 384.202 192.101 7.35 0.019
Square 2 489.82 489.816 244.908 9.37 0.010
Interaction 1 4.10 4.098 4.098 0.16 0.704
Residual Error 7 182.89 182.892 26.127
Lack-of-Fit 3 127.75 127.753 42.584 3.09 0.152
Pure Error 4 55.14 55.139 13.785
Total 12 1062.29

Obs StdOrder Y*Q Fit SE Fit Residual St Resid


1 4 36.754 35.082 4.041 1.671 0.53
2 5 20.640 16.999 4.041 3.640 1.16
3 3 20.568 25.209 4.041 -4.641 -1.48
4 1 16.005 16.030 4.041 -0.025 -0.01
5 9 36.908 39.116 2.286 -2.208 -0.48
6 10 35.463 39.116 2.286 -3.654 -0.80
7 8 35.225 32.784 4.041 2.441 0.78
8 2 36.240 29.952 4.041 6.288 2.01 R
9 12 44.377 39.116 2.286 5.260 1.15
10 13 37.288 39.116 2.286 -1.828 -0.40
11 7 18.577 22.665 4.041 -4.088 -1.31
12 11 41.545 39.116 2.286 2.429 0.53
13 6 28.537 33.825 4.041 -5.287 -1.69

R denotes an observation with a large standardized residual.

Remove Standard Order 2.

Response Surface Regression: Y*Q versus Temp, C, Time, min

The analysis was done using uncoded units.

Estimated Regression Coefficients for Y*Q

Term Coef SE Coef T P


Constant -498.713 99.8349 -4.995 0.002
Temp, C 1.610 0.3000 5.365 0.002
Time, min 0.517 0.4693 1.103 0.312
Temp, C*Temp, C -0.001 0.0003 -5.600 0.001
Time, min*Time, min -0.004 0.0009 -4.780 0.003
Temp, C*Time, min 0.001 0.0008 1.371 0.219

S = 3.59288 PRESS = 318.747


R-Sq = 92.53% R-Sq(pred) = 69.26% R-Sq(adj) = 86.31%

Analysis of Variance for Y*Q

Source DF Seq SS Adj SS Adj MS F P


Regression 5 959.40 959.40 191.88 14.86 0.003
Linear 2 369.14 371.70 185.85 14.40 0.005
Square 2 565.99 590.20 295.10 22.86 0.002
Interaction 1 24.27 24.27 24.27 1.88 0.219
Residual Error 6 77.45 77.45 12.91
Lack-of-Fit 2 22.31 22.31 11.16 0.81 0.507
Pure Error 4 55.14 55.14 13.78
Total 11 1036.85

50
Obs StdOrder Y*Q Fit SE Fit Residual St Resid
1 4 36.754 37.178 2.934 -0.425 -0.20
2 5 20.640 17.867 2.857 2.772 1.27
3 3 20.568 23.113 2.934 -2.545 -1.23
4 1 16.005 18.126 2.934 -2.121 -1.02
5 9 36.908 39.116 1.607 -2.208 -0.69
6 10 35.463 39.116 1.607 -3.654 -1.14
7 8 35.225 33.652 2.857 1.573 0.72
8 12 44.377 39.116 1.607 5.260 1.64
9 13 37.288 39.116 1.607 -1.828 -0.57
10 7 18.577 17.605 3.347 0.972 0.74
11 11 41.545 39.116 1.607 2.429 0.76
12 6 28.537 28.764 3.347 -0.227 -0.17

Remove Temp*Time.

Response Surface Regression: Y*Q versus Temp, C, Time, min

The analysis was done using uncoded units.

Estimated Regression Coefficients for Y*Q

Term Coef SE Coef T P


Constant -554.997 96.5560 -5.748 0.001
Temp, C 1.677 0.3139 5.343 0.001
Time, min 1.090 0.2275 4.790 0.002
Temp, C*Temp, C -0.001 0.0003 -5.136 0.001
Time, min*Time, min -0.004 0.0009 -4.352 0.003

S = 3.81203 PRESS = 327.774


R-Sq = 90.19% R-Sq(pred) = 68.39% R-Sq(adj) = 84.58%

Analysis of Variance for Y*Q

Source DF Seq SS Adj SS Adj MS F P


Regression 4 935.13 935.131 233.783 16.09 0.001
Linear 2 369.14 640.551 320.276 22.04 0.001
Square 2 565.99 565.991 282.996 19.47 0.001
Residual Error 7 101.72 101.721 14.532
Lack-of-Fit 3 46.58 46.582 15.527 1.13 0.438
Pure Error 4 55.14 55.139 13.785
Total 11 1036.85

Obs StdOrder Y*Q Fit SE Fit Residual St Resid


1 4 36.754 34.634 2.411 2.119 0.72
2 5 20.640 17.604 3.024 3.036 1.31
3 3 20.568 25.657 2.411 -5.089 -1.72
4 1 16.005 15.582 2.411 0.423 0.14
5 9 36.908 39.116 1.705 -2.208 -0.65
6 10 35.463 39.116 1.705 -3.654 -1.07
7 8 35.225 33.389 3.024 1.836 0.79
8 12 44.377 39.116 1.705 5.260 1.54
9 13 37.288 39.116 1.705 -1.828 -0.54
10 7 18.577 19.140 3.347 -0.563 -0.31
11 11 41.545 39.116 1.705 2.429 0.71
12 6 28.537 30.300 3.347 -1.762 -0.97

51
Response Surface Regression: Y*Q versus Temp, C, Time, min

The analysis was done using coded units.

Estimated Regression Coefficients for Y*Q

Term Coef SE Coef T P


Constant 39.116 1.705 22.945 0.000
Temp, C 4.489 1.476 3.040 0.019
Time, min 5.037 1.476 3.412 0.011
Temp, C*Temp, C -7.582 1.476 -5.136 0.001
Time, min*Time, min -6.426 1.476 -4.352 0.003

S = 3.81203 PRESS = 327.774


R-Sq = 90.19% R-Sq(pred) = 68.39% R-Sq(adj) = 84.58%

Analysis of Variance for Y*Q

Source DF Seq SS Adj SS Adj MS F P


Regression 4 935.13 935.131 233.783 16.09 0.001
Linear 2 369.14 363.848 181.924 12.52 0.005
Square 2 565.99 565.991 282.996 19.47 0.001
Residual Error 7 101.72 101.721 14.532
Lack-of-Fit 3 46.58 46.582 15.527 1.13 0.438
Pure Error 4 55.14 55.139 13.785
Total 11 1036.85

Obs StdOrder Y*Q Fit SE Fit Residual St Resid


1 4 36.754 34.634 2.411 2.119 0.72
2 5 20.640 17.604 3.024 3.036 1.31
3 3 20.568 25.657 2.411 -5.089 -1.72
4 1 16.005 15.582 2.411 0.423 0.14
5 9 36.908 39.116 1.705 -2.208 -0.65
6 10 35.463 39.116 1.705 -3.654 -1.07
7 8 35.225 33.389 3.024 1.836 0.79
8 12 44.377 39.116 1.705 5.260 1.54
9 13 37.288 39.116 1.705 -1.828 -0.54
10 7 18.577 19.140 3.347 -0.563 -0.31
11 11 41.545 39.116 1.705 2.429 0.71
12 6 28.537 30.300 3.347 -1.762 -0.97

Estimated Regression Coefficients for Y*Q using data in uncoded units

Term Coef
Constant -554.997
Temp, C 1.67738
Time, min 1.08982
Temp, C*Temp, C -0.00134794
Time, min*Time, min -0.00401616

52
D.3. Calculation of Optimum Temperature, Time and Y*Q
𝑌 ∗ 𝑄 = −554.997 + 1.6774𝑇 + 1.0898𝑡 − 0.00135𝑇 2 − 0.000402𝑡 2
𝑑(𝑌 ∗ 𝑄)
= 0 = 1.6774 − 2(0.00135)𝑇
𝑑𝑇
𝑑(𝑌 ∗ 𝑄)
= 0 = 1.0898 − 2(0.00402)𝑡
𝑑𝑡
Topt = 621.26 °C
topt = 135.55 mins
Y*Qopt = 39.913 mg removed pollutant per gram dried material

53
APPENDIX E

MATERIALS AND EQUIPMENT

54
Appendix E

Materials and Equipment

Sartorius Analytical Balance 210S (BL210S)

Clay Adams® Compact II Centrifuge

55
Scientific Oven 1 Series 2000

Thermo Scientific MaxQ™ 2000 Water Bath Shaker

56
Hitachi U-5100 UV-Vis Spectrophotometer

Fisher Scientific Furnace

57

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