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SCHOOL OF INDUSTRIAL TECHNOLOGY

SEMESTER II

ACADEMIC SESSION 2019/2020

IUK 208-EXPERIMENTAL DESIGN WITH COMPUTER


APPLICATION

PROCESS OPTIMIZATION USING DESIGN-EXPERT®


STATISTICAL SOFTWARE

LECTURER : DR. TAN JOO SHUN

NAME : NURUL HIDAYAH BINTI KAMARUZAMAN


MATRIC NUMBER : 142189
DIVISON : FOOD TECHNOLOGY

SUBMISSION DATE: 15 MAY 2020


1) Students need to prepare a report with the design matrix, predicted response, ANOVA, final
equation, 3D plots with significant interaction effect between factors, constraints of the factors and
response and a suggested solution.

DESIGN MATRIX

Table 1: Central composite design on a fermentation process

Factor 1 Factor 2 Factor 3 Response 1


Std Block Run Space Type A:CATALYST B:CHITIN C:NaOH CHITOSAN YIELD
g/L g/L % g/L
1 Block 1 19 Factorial 3 20 20 69
2 Block 1 11 Factorial 10 20 20 139
3 Block 1 15 Factorial 3 60 20 188
4 Block 1 6 Factorial 10 60 20 189
5 Block 1 12 Factorial 3 20 60 259
6 Block 1 18 Factorial 10 20 60 93
7 Block 1 7 Factorial 3 60 60 334
8 Block 1 20 Factorial 10 60 60 141
9 Block 1 16 Axial 0.613725 40 40 235
10 Block 1 4 Axial 12.3863 40 40 153
11 Block 1 3 Axial 6.5 6.36414 40 129
12 Block 1 9 Axial 6.5 73.6359 40 251
13 Block 1 8 Axial 6.5 40 6.36414 60
14 Block 1 2 Axial 6.5 40 73.6359 165
15 Block 1 1 Center 6.5 40 40 289
16 Block 1 14 Center 6.5 40 40 304
17 Block 1 10 Center 6.5 40 40 319
18 Block 1 17 Center 6.5 40 40 309
19 Block 1 5 Center 6.5 40 40 316
20 Block 1 13 Center 6.5 40 40 303
PREDICTED RESPOND

Report

Table 2: Predicted value of experimental response chitosan

Influence
Internally Externally
Run Actual Predicted Cook's on Fitted Standard
Residual Leverage Studentized Studentized
Order Value Value Distance Value Order
Residuals Residuals
DFFITS
1 289.00 306.03 -17.03 0.166 -1.187 -1.215 0.028 -0.543 15
2 165.00 175.09 -10.09 0.607 -1.025 -1.027 0.162 -1.278 14
3 129.00 139.82 -10.82 0.607 -1.098 -1.111 0.187 -1.382 11
4 153.00 152.60 0.4040 0.607 0.041 0.039 0.000 0.048 10
5 316.00 306.03 9.97 0.166 0.694 0.675 0.010 0.302 19
6 189.00 190.76 -1.76 0.670 -0.195 -0.185 0.008 -0.263 4
7 334.00 326.93 7.07 0.670 0.782 0.766 0.124 1.091 7
8 60.00 72.00 -12.00 0.607 -1.218 -1.252 0.229 -1.557 13
9 251.00 262.27 -11.27 0.607 -1.144 -1.164 0.202 -1.448 12
10 319.00 306.03 12.97 0.166 0.903 0.894 0.016 0.399 17
11 139.00 130.45 8.55 0.670 0.947 0.941 0.182 1.341 2
12 259.00 241.62 17.38 0.670 1.924 2.300 0.751 3.275⁽¹⁾ 5
13 303.00 306.03 -3.03 0.166 -0.211 -0.201 0.001 -0.090 20
14 304.00 306.03 -2.03 0.166 -0.142 -0.135 0.000 -0.060 16
15 188.00 169.63 18.37 0.670 2.034 2.519 0.839 3.587⁽¹⁾ 3
16 235.00 257.49 -22.49 0.607 -2.284 -3.132 0.806 -3.894⁽¹⁾ 9
17 309.00 306.03 2.97 0.166 0.207 0.196 0.001 0.088 18
18 93.00 95.75 -2.75 0.670 -0.304 -0.290 0.019 -0.413 6
19 69.00 61.32 7.68 0.670 0.850 0.837 0.147 1.192 1
20 141.00 133.06 7.94 0.670 0.879 0.868 0.157 1.236 8
ANOVA for Quadratic model

Response 1: CHITOSAN YIELD

Table 3: ANOVA table

Source Sum of Squares df Mean Square F-value p-value


Model 1.528E+05 9 16976.31 68.70 < 0.0001 significant
A-CATALYST 13282.47 1 13282.47 53.75 < 0.0001
B-CHITIN 18099.83 1 18099.83 73.25 < 0.0001
C-NaOH 12829.90 1 12829.90 51.92 < 0.0001
AB 1152.00 1 1152.00 4.66 0.0562
AC 23112.50 1 23112.50 93.54 < 0.0001
BC 264.50 1 264.50 1.07 0.3252
A² 18372.58 1 18372.58 74.35 < 0.0001
B² 19856.80 1 19856.80 80.36 < 0.0001
C² 59991.72 1 59991.72 242.79 < 0.0001
Residual 2470.93 10 247.09
Lack of Fit 1893.60 5 378.72 3.28 0.1092 not significant
Pure Error 577.33 5 115.47
Cor Total 1.553E+05 19

Factor coding is Coded.


Sum of squares is Type III - Partial

The Model F-value of 68.70 implies the model is significant. There is only a 0.01% chance that an F-
value this large could occur due to noise.

P-values less than 0.0500 indicate model terms are significant. In this case A, B, C, AC, A², B², C² are
significant model terms. Values greater than 0.1000 indicate the model terms are not significant. If
there are many insignificant model terms (not counting those required to support hierarchy), model
reduction may improve your model.

The Lack of Fit F-value of 3.28 implies the Lack of Fit is not significant relative to the pure error.
There is a 10.92% chance that a Lack of Fit F-value this large could occur due to noise. Non-significant
lack of fit is good.
Fit Statistics

Table 4: Fit Statistic

Std. Dev. 15.72 R² 0.9841


Mean 212.25 Adjusted R² 0.9698
C.V. % 7.41 Predicted R² 0.9002
Adeq Precision 23.8963

R2 is near to 1.0 indicates it is good and well fit to the model. The Predicted R² of 0.9002 is in
reasonable agreement with the Adjusted R² of 0.9698; i.e. the difference is less than 0.2.

Adeq Precision measures the signal to noise ratio. A ratio greater than 4 is desirable. Ratio of 23.896
indicates an adequate signal. This model can be used to navigate the design space.

Coefficients in Terms of Coded Factors

Table 5: Coefficient

Factor Coefficient Estimate df Standard Error 95% CI Low 95% CI High VIF
Intercept 306.03 1 6.41 291.75 320.32
A-CATALYST -31.19 1 4.25 -40.66 -21.71 1.0000
B-CHITIN 36.41 1 4.25 26.93 45.88 1.0000
C-NaOH 30.65 1 4.25 21.17 40.13 1.0000
AB -12.00 1 5.56 -24.38 0.3831 1.0000
AC -53.75 1 5.56 -66.13 -41.37 1.0000
BC -5.75 1 5.56 -18.13 6.63 1.0000
A² -35.71 1 4.14 -44.93 -26.48 1.02
B² -37.12 1 4.14 -46.35 -27.89 1.02
C² -64.52 1 4.14 -73.75 -55.29 1.02

A (catalyst) have negative effect to the yield while B (chitin) and C (NaOH) have positive effect to the
yield. The interaction of A and C is not a good combination because it has negative effect toward the
yield. A and C will reduce the chitosan yield if combined together.
Final Equation in Terms of Coded Factors

Table 6: Final Equation

CHITOSAN YIELD =
+306.03
-31.19 A
+36.41 B
+30.65 C
-12.00 AB
-53.75 AC
-5.75 BC
-35.71 A²
-37.12 B²
-64.52 C²

Chitosan Yield= 306.035 + -31.1863 * A + 36.4051 * B + 30.6504 * C + -12 * AB + -53.75 * AC + -


5.75 * BC + -35.7054 * A^2 + -37.1196 * B^2 + -64.52 * C^2

3D Plots with Significant Interaction Effect between Factors


From the graph, the interaction effect of A and C is shown. When less catalyst and more NaOH
concentration added, the maximum chitosan yield is obtained. The red region on the graph is the
highest chitosan yield. So it is better to use low concentration of catalyst and high concentration of
NaOH to get maximum chitosan yield.

Constraints

Table 7: Constraints

Name Goal Lower Limit Upper Limit Lower Weight Upper Weight Importance
A:CATALYST is in range 3 10 1 1 3
B:CHITIN is in range 20 60 1 1 3
C:NaOH is in range 20 60 1 1 3
CHITOSAN YIELD maximize 60 334 1 1 3

With this constraints, 100 solutions are obtained.

Solutions

Table 8: 5 from 100 solutions obtained

Number CATALYST CHITIN NaOH CHITOSAN YIELD Desirability


1 3.472 56.961 51.109 339.512 1.000 Selected
2 4.644 48.026 47.171 335.807 1.000
3 3.606 44.169 48.234 334.941 1.000
4 3.947 56.949 45.350 334.164 1.000
5 3.556 43.043 51.217 334.981 1.000

The suggested solution is catalyst: 3.472 g/L, chitin: 56.961 g/L and NaOH: 51.109% which will
give chitosan yield of 339.512 g/L with desirability of 1.0.

2) What are the optimum conditions to obtain the maximum yield of chitosan at minimum cost?

To obtain the maximum yield of chitosan at minimum cost, optimization is conducted and all the
factors is minimized and the chitosan yield is maximized.
Constraints

Name Goal Lower Limit Upper Limit Lower Weight Upper Weight Importance
A:CATALYST minimize 3 10 1 1 3
B:CHITIN minimize 20 60 1 1 3
C:NaOH minimize 20 60 1 1 3
CHITOSAN YIELD maximize 60 334 1 1 3

Solutions

13 Solutions found to get maximum chitosan yield at minimum cost.

Number CATALYST CHITIN NaOH CHITOSAN YIELD Desirability


1 3.000 26.961 34.142 222.823 0.751 Selected
2 3.000 26.931 34.144 222.692 0.751
3 3.000 27.152 34.133 223.707 0.751
4 3.000 26.766 34.289 222.788 0.751
5 3.000 26.963 33.959 221.688 0.751
6 3.000 26.540 34.290 221.668 0.750
7 3.000 26.848 34.614 225.208 0.750
8 3.000 27.615 33.611 222.629 0.750
9 3.000 26.567 34.818 225.061 0.750
10 3.036 26.867 34.119 222.871 0.750
11 3.000 27.273 36.459 238.073 0.748
12 3.615 28.760 33.119 235.194 0.744
13 3.000 37.623 26.519 208.574 0.710

3) In the validation experiment, 256 g/L, 270 g/L and 265 g/L of chitosan yield was obtained in
triplicate runs. Is the model valid in this study?

Confirmation

Two-sided Confidence = 95%

Predicted Predicted 95% PI Data 95% PI


Response Observed Std Dev n SE Pred
Mean Median low Mean high
CHITOSAN
222.804 222.804 15.7192 3 12.1474 195.738 263.667 249.87
YIELD
The model is not valid in this study. The predicted mean (222.804) have a large difference with data
mean (263.667). ± 5% from the predicted mean is considered as normal and valid in this study.

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