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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).
1
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.
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.
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.
2
1.4 Plan of Investigation
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.
3
CHAPTER 2
2.1 Breadnut
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
4
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).
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).
5
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).
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).
6
CHAPTER 3
METHODOLOGY
3.1 Equipment
3.2 Reagents
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.
7
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:
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.
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.
8
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).
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.
9
Chapter 4
This chapter presents the analyses of the data gathered from the experiment.
Also, relevant data are presented in this chapter.
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.
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
10
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
11
Obs StdOrder Yield Fit SE Fit Residual St Resid
Table 4.3. Final Response Surface Regression: Yield versus temp, time
12
S = 2.17112 PRESS = 125.035
R-Sq = 91.47% R-Sq(pred) = 62.27% R-Sq(adj) = 85.78%
Term Coef
Constant -502.276
temp 1.67628
time 0.487049
temp*temp -0.00137529
time*time -0.00203291
13
From the estimated regression coefficients for yield, the data suggested a
correlation of:
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.
After obtaining the optimum time and temperature, the values were substituted to
the equation:
14
4.2 Determination of Adsorption Capacity
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.
15
Table 4.5. Initial Response Surface Regression: Adsorption Capacity versus temp,
time
16
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
17
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
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
18
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.
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
The Qopt that was estimated is 125.174 milligram of MB per gram of activated carbon.
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.
19
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
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
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
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.
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
Based on the analyses drawn together, the research proved that breadnut peels
can be an alternative raw material for preparation of activated carbon.
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:
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.
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.
26
Bibliography
BASF Chemical Company (2012). "The birth of the chemical industry and the era of
dyes." from http://www.basf.com/group/corporate/en/about-basf/history/1865-
1901/index.
Foust, A., L. Wenzel, C. Clump, L. Maus and L. B. Andersen (1980). Principles of Unit
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.
27
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."
ScienceDirect- Desalination(238): 210-232.
Ozer, A. and G. Dursun (2007). "Removal of methylene blue from aqueous solution by
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.
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.
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
30
APPENDIX A
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
31
A.3 Calibration Curve
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
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
(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
(250 − 0.3760)(0.0514)
𝑄=
(0.1208)
Q = 124.8120 mg/g
33
APPENDIX B
34
APPENDIX B
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
35
S = 4.79003 PRESS = 835.805
R-Sq = 68.42% R-Sq(pred) = 0.00% R-Sq(adj) = 45.86%
Remove Temp*time
36
Analysis of Variance for Yield
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
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
Term Coef
Constant -502.276
temp 1.67628
time 0.487049
temp*temp -0.00137529
time*time -0.00203291
39
APPENDIX C
40
APPENDIX C
41
Analysis of Variance for Q
42
Analysis of Variance for Q
43
Analysis of Variance for Q
Remove Time*Time
44
Analysis of Variance for Q
45
Analysis of Variance for Q
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
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
47
APPENDIX D
48
APPENDIX D
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
49
Analysis of Variance for Y*Q
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.
51
Response Surface Regression: Y*Q versus Temp, C, Time, min
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
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APPENDIX E
54
Appendix E
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Scientific Oven 1 Series 2000
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Hitachi U-5100 UV-Vis Spectrophotometer
57