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Response Surface
Methodology (RSM)
Present by:
Wan Nor Nadyaini Wan Omar,
B.Eng (Chem),M.Eng (Chem)
Faculty of Chemical Engineering
(wnnadyaini@gmail.com)
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IF??
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Research Cycle process
Ask Question:
Objective of study
Experimental
Graphical analysis
Design
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DATA COLLECTION
To clarify the objective of experiment
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What is DOE?
A collection of predetermined process variables
setting
What is RSM?
Response Surface Methodology (RSM) is a statistic
techniques employed a regression analysis to
performed for the collective data.
What is STATISTICA, Design Expert, MiniTab
and etc?
• is a tools to help we designs our experiment and
analyses our data.
• RSM is one of the technique that have been programmed
in that software.
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What DOE & RSM can do?
PREDICTION OPTIMIZATION
Mathematical model
Find relationship
Optimization
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Step in RSM study
Before: Select the
variable-Design the
experiment
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Before Experiment
PROCESS •Which factor are most important and therefore will be included in the
experiment, and which are least important and can these factor be
VARIABLE omitted? With the important factors, can the desired effects be detected?
EXPERIMENTAL •What is the experimental unit, that is to say, what is the piece of
experimental material from which a response value is measured? How
UNIT are the experimental units to be replicated, if at all?
•The choice of the factors and level determined the type, size and
DESICION experimental region. The no. of level at each factor as well as the no. of
replicated experiment units represent the total no. of experiment.
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Design of experiment
(DOE) Process
Type of design
• Full factorial
Factor • Fractional factorial
• No of • Placket Burman
Independent • CCD
Var. • Box-behnken
Objective
• Block • Taguchi
• Screening • Level • Etc.
• Prediction • Range
• Optimization
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Objective
Screening
Optimization
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1) Selecting the Parameter
Factors:
Responses:
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2) Selecting the Level
Two level (2k) - (-1,+1)-first order,
• Two-level factorial design is each factor is evaluated at a “low”
setting and at “high” setting.
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Experimental region
o The region of conceivable factor level values that represents
the factor combinations of potential interest.
o Need to determined before the experiment by finding the
range of variables.
o If at the end of analysis, the factor value or optimum is out of
the range, the experiment need to repeat with the new
range.
Range and Levels
Factors Symbol
-1 0 +1
Molar ratio methanol: oil X1 20:1 30:1 40:1
Catalyst loading, wt% X2 2 3 4
Reaction Time, min X3 120 180 240
Reaction Temperature X4 90 120 150
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3) Selecting the Type of
DOE
• Full factorial
• Fractional factorial The most
• Placket Burman popular is CCD
• CCD and box-
• Box-behnken behnken design
• Taguchi
• Etc.
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Factorial design
Easy to be used by simply following relatively simple design
Able to meet the majority of the experimental needs and its data
analysis can be performed by graphical methods
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Full factorial & fractional
factorial
• Two level Full factorial (-1,+1)= 2k Rotatable
• Three level full factorial (-1,0,+1) =3k
• Fractional factorial (two level) = 2k-m, m<k
o ½= 2k-1
o 1/4= 2k-2
Orthogonal
o 1/8= 2k-4
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Matrix Arrangement
(2-level)
2-level factorial design (full)
2-level fractional fractorial design A B C D
(resolution IV) 1 -1 -1 -1 -1
2 1 -1 -1 -1
3 -1 1 -1 -1
A B C D 4 1 1 -1 -1
1 -1 -1 -1 -1 5 -1 -1 1 -1
2 1 -1 -1 1 6 1 -1 1 -1
3 -1 1 -1 1 7 -1 1 1 -1
4 1 1 -1 -1 8 1 1 1 -1
5 -1 -1 1 1 9 -1 -1 -1 1
6 1 -1 1 -1 10 1 -1 -1 1
7 -1 1 1 -1 11 -1 1 -1 1
8 1 1 1 1 12 1 1 -1 1
13 -1 -1 1 1
14 1 -1 1 1
15 -1 1 1 1
16 1 1 1 1
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Matrix Arrangement
(3-level) 3**(4-1) fractional factorial design, 9 3**(4-1) fractional factorial
3**(4-1) fractional factorial
design, 1 block , 27 runs
3**(4-0) full factorial design, 1 block , blocks, 27 runs (Spreadsheet1) design, 3 blocks, 27 runs
(Spreadsheet1)
81 runs (Spreadsheet1) Bloc (Spreadsheet1)
A B C D A B C D
A B C D k
Block A B C D 1 -1 -1 -1 -1
1 -1 -1 -1 -1 1 1 0 1 0 1
1 1 1 0 -1 -1 2 -1 -1 0 1
2 -1 -1 -1 0 2 1 1 0 1 0
2 1 0 1 0 1 3 -1 -1 1 0
3 -1 -1 -1 1 5 2 1 0 0 1
4 -1 -1 0 -1 3 1 -1 -1 0 1 4 -1 0 -1 1
6 2 0 1 -1 -1
5 -1 -1 0 0 5 -1 0 0 0
7 3 1 0 -1 -1 4 1 0 1 -1 -1
6 -1 -1 0 1 6 -1 0 1 -1
8 3 -1 -1 0 1 5 1 1 0 0 1
7 -1 -1 1 -1 7 -1 1 -1 0
11 4 -1 0 -1 1 6 1 -1 -1 1 0
8 -1 -1 1 0 8 -1 1 0 -1
12 4 1 1 1 -1 13 2 0 -1 1 -1
67 1 0 0 -1 9 -1 1 1 1
68 1 0 0 0 13 5 -1 0 1 -1 14 2 0 -1 0 0
10 0 -1 -1 1
69 1 0 0 1 14 5 1 1 0 0 15 2 0 -1 -1 1
11 0 -1 0 0
70 1 0 1 -1 15 5 0 -1 -1 1 16 2 1 1 0 0
12 0 -1 1 -1
71 1 0 1 0 16 6 1 1 -1 1 17 2 -1 0 -1 1
72 1 0 1 1 18 0 1 1 0
17 6 0 -1 1 -1 18 2 1 1 1 -1
73 1 1 -1 -1 19 1 -1 -1 0
18 6 -1 0 0 0
74 1 1 -1 0 19 3 0 0 1 1 20 1 -1 0 -1
19 7 -1 1 -1 0
75 1 1 -1 1 20 3 0 0 0 -1 21 1 -1 1 1
20 7 0 0 0 -1
76 1 1 0 -1 21 3 -1 1 -1 0 22 1 0 -1 -1
21 7 1 -1 1 1
77 1 1 0 0 22 3 0 0 -1 0 23 1 0 0 1
78 1 1 0 1 22 8 0 0 -1 0
23 3 1 -1 1 1 24 1 0 1 0
79 1 1 1 -1 23 8 1 -1 0 -1
24 3 1 -1 0 -1 25 1 1 -1 1
80 1 1 1 0 24 8 -1 1 1 1
25 3 1 -1 -1 0 26 1 1 0 0
81 1 1 1 1 25 9 0 0 1 1
26 3 -1 1 1 1 27 1 1 1 -1
26 9 1 -1 -1 0
27 3 -1 1 0 -1
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Central Composite Design
(CCD)
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Box-behnken design
The equivalent in the case of 3(k-p) designs (3-level full factorial with
incomplete block) are the so-called Box-Behnken designs (Box and
Behnken, 1960).
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DOE Matrix Arrangement
-1.00 -1.00 -1.00 -1.00 -1.00 -1.00 -1.00 -1.00 -1.00 -1.00 0.00 0.00
-1.00 -1.00 -1.00 1.00 -1.00 -1.00 0.00 1.00 1.00 -1.00 0.00 0.00
-1.00 -1.00 1.00 -1.00 -1.00 -1.00 1.00 0.00 -1.00 1.00 0.00 0.00
-1.00 -1.00 1.00 1.00 -1.00 0.00 -1.00 1.00 1.00 1.00 0.00 0.00
-1.00 1.00 -1.00 -1.00 -1.00 0.00 0.00 0.00 0.00 0.00 -1.00 -1.00
-1.00 1.00 -1.00 1.00 -1.00 0.00 1.00 -1.00 0.00 0.00 1.00 -1.00
-1.00 1.00 1.00 -1.00 -1.00 1.00 -1.00 0.00 0.00 0.00 -1.00 1.00
-1.00 1.00 1.00 1.00 -1.00 1.00 0.00 -1.00 0.00 0.00 1.00 1.00
1.00 -1.00 -1.00 -1.00 -1.00 1.00 1.00 1.00 0.00 0.00 0.00 0.00
1.00 -1.00 -1.00 1.00 0.00 -1.00 -1.00 1.00 -1.00 0.00 0.00 -1.00
1.00 -1.00 1.00 -1.00 0.00 -1.00 0.00 0.00 1.00 0.00 0.00 -1.00
1.00 -1.00 1.00 1.00 0.00 -1.00 1.00 -1.00 -1.00 0.00 0.00 1.00
1.00 1.00 -1.00 -1.00 0.00 0.00 -1.00 0.00 1.00 0.00 0.00 1.00
1.00 1.00 -1.00 1.00 0.00 0.00 0.00 -1.00 0.00 -1.00 -1.00 0.00
1.00 1.00 1.00 -1.00 0.00 0.00 1.00 1.00 0.00 1.00 -1.00 0.00
1.00 1.00 1.00 1.00 0.00 1.00 -1.00 -1.00 0.00 -1.00 1.00 0.00
-2.00 0.00 0.00 0.00 0.00 1.00 0.00 1.00 0.00 1.00 1.00 0.00
2.00 0.00 0.00 0.00 0.00 1.00 1.00 0.00 0.00 0.00 0.00 0.00
0.00 -2.00 0.00 0.00 1.00 -1.00 -1.00 0.00 -1.00 0.00 -1.00 0.00
0.00 2.00 0.00 0.00 1.00 -1.00 0.00 -1.00 1.00 0.00 -1.00 0.00
0.00 0.00 -2.00 0.00 1.00 -1.00 1.00 1.00 -1.00 0.00 1.00 0.00
0.00 0.00 2.00 0.00 1.00 0.00 -1.00 -1.00 1.00 0.00 1.00 0.00
0.00 0.00 0.00 -2.00 1.00 0.00 0.00 1.00 0.00 -1.00 0.00 -1.00
0.00 0.00 0.00 2.00 1.00 0.00 1.00 0.00 0.00 1.00 0.00 -1.00
0.00 0.00 0.00 0.00 1.00 1.00 -1.00 1.00 0.00 -1.00 0.00 1.00
0.00 0.00 0.00 0.00 1.00 1.00 0.00 0.00 0.00 1.00 0.00 1.00
1.00 1.00 1.00 -1.00 0.00 0.00 0.00 0.00
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CCD, 26 run 3 fractional factorial, 27 run BBD, 27 run
CCD vs BBD
Criteria CCD BBD
Design 2-level factorial, with 3-level fractional
star point factorial,
Block Up to researcher Limited
Mean effect Not considered Considered
Interaction Linear Linear, quadratic
Optimization Yes Yes
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DOE Table
Run Manipulated Variables Response
s X1 X2 X3 s
Operating Level Molar Ratio Level Reaction Level Yield, Y1
temperature,T(oC b (meOH: oil) b time,t (h) b (%)
)
1 50 -1 3 -1 2 -1 91.90
2 50 -1 3 -1 4 +1 84.60
3 50 -1 10 +1 2 -1 65.15
4 50 -1 10 +1 4 +1 95.95
5 70 +1 3 -1 2 -1 63.90
6 70 +1 3 -1 4 +1 94.95
7 70 +1 10 +1 2 -1 87.60
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Addition note
Randomisation
Replication
• Repetition of experiments
• It is essential feature to increase the degree of belief
Blocking
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1. Insert the complete data into DOE
2. Develop the empirical/predicted model
3. Statistic analysis of empirical model
4. Find the importance of process variables
5. Investigate the influence of process variables
6. Optimization of process variables
After experiment
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1) Complete data
Insert the collected data into the software.
(refer to tutorial 2)
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• First Order polynomial
• Second Order polynomial
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Second order model
(polynomial)
• Normally used for optimization since it is consider
the center point.
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• Regression analysis
• ANOVA
• Hypothesis testing
3) Statistic analysis of
model
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Validity of model
The adequacy of the fitted model is checked
by ANOVA (Analysis of Variance) using
Fisher F-test
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Observed and predicted
table
Yu
Ŷu
Ÿ=mean
SSR=∑(Ŷu- Ÿ )2=4.4225
SSR=
The value of 0, indicated that none of the variability in the data can be
explained by predicted model.
R2 is closer to 1, the
predicted model is more
reliable R2>0.75 acceptable
(Haaland), however, >0.8
is much better
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Analysis of variance (ANOVA)
• The F-value is a measurement of variance of data about
the mean based on the ratio of mean square (MS) of
group variance due to error.
• F table =F(p−1,N−p,α)
o p−1 :DFregression
o N−p:DFresidual
o N=total exp
o P=no of term in fitted model
o α-value: level of significant
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Hypothesis testing (F value)
• There are 2 statement is comparing at significant
confident level (95%, α= 0.05) F table Can be
find online
4) Importance/significant of
process variables
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Significant of the model coefficient
TValue:
Pvalue
Can be visualized
• Pareto Chart
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plot 44
Interpretation?
- If a p-value is ≤ 0.01, then the Ho can be rejected at a 1%
significance level “convincing” evidence that the HA is true.
5) Interaction/influence of
process variables
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Visualize the result
• Predicted response function (Ŷ) (read “Y hat”):
o Predict the value of response
• Response surface:
o Represent the relationship between predicted response function and
factor
o Is visualized in 3D, contour, single parameter;
105
100
95
90
Lignin Degradation (%)
85
80
75
70
65
60
55
.25 .63
Particle size (mm)
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Single Variables
• The graph is plot the predicted Mean of value of
process variables
100
105
100 95
95
90
90
Lignin Degradation (%)
85
85
%
80
75 80
70
75
65
Lignin degradation (%)
Gluc os e rec ov ery (%)
60 70
55
.25 .63
65
Particle size (mm) 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
Partic le Siz e (mm)
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Contour
Visualized the shape of the 3D response surface
Line or curves (known as contour) represent the surface of response value are
drawn on graph or plane whose coordinates represent the level of the factor.
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Examples (Ellipse)
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Examples (saddle point)
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Example (Circular)
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3D surface plot
Shows the interaction between two
process variables as function of factors.
Shape
•Minimum: basin
•Maximum: hill
•Saddle: saddle shape
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Surface
Parabola, maximum hill
Saddle-shaped
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Quadratic interaction
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How to interpret? 3
Stationary point
2
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6) Optimization
• Single response
• Multi response
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Optimization: Single
response-Critical value
Will identified the point on the quadratic response surface
either it the minimum, maximum, or saddle point of the
surface.
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OPTIMIZATION: Multi-response via
Desirability Function
A popular and established technique for simultaneous
determization of optimum settings of input variables that can
determine optimum performance levels for one or more
responses
Predicted
value
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Contour plot
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Conclusion
DOE and RSM
• A powerful method for design of experimentation,
analysis of experimental data, and optimization.
Advantages
• design of experiment, statistical analysis, optimization,
and profile of analysis in one step
• Produce empirical mathematical model
Disadvantage
• The prediction only can be determined in range of
study.
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references
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Slide can be found at
https://teknologimalaysia.academia.edu/DahliaOmar
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Statistica Tutorial 1
DESIGN OF EXPERIMENT
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DOE spreadsheet
Open spreadsheet STEP 1
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STEP 3 Click industrial statistics & six
sigma
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Design & analysis of experiment windows
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CCD
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STEP 7 Click change factor value etc
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Change value
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STEP 9
Click design display
(standard order)
Design display on
workbook windows
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Copy DOE to spreedsheet
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Edit, save & print spreedsheet
STEP 1 Right click on the
column→edit
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Statistica tutorial 2
INSERT AND ANALYSIS THE DATA
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Insert the result into
spreadsheet
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STEP 2 Click Statistica
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STEP 5 Click central composite, non factorial, surface
design→ok
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STEP 8 Click variables
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STEP 9 Pick variable →ok
STEP 10 Click ok
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Analysis of the central composite (response surface) experiment windows opened.
(note: this windows is an important for analysis since it display all information
needed)
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Save as project
This statistica project file can be opened anytime and the analysis and workbook
could be resume.
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STATISTICA TUTORIAL 3
PREDICTED/EMPIRICAL MODEL
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Model (Coefficient
selection)
STEP 1
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STEP 2 Click Anova/effect
→regression coefficient
2 2 2 2
Y2 = −192.048 + 4.623X 1 − 0.266X 2 + 0.774X 3 + 1.978X 4 − 0.050X 1 − 0.843X 2 − 0.001X 3 − 0.003X 4
− 0.198X 1 X 2 + 0.004X 1 X 3 − 0.011X 1 X 4 + 0.056X 2 X 3 + 0.001X 2 X 4 − 0.005X 3 X 4
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STATISTICA TUTORIAL 4
ANOVA
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ANOVA/Effects
Residual
DF SST
Regression
2807.32 14 200.52 3.39 >2.74
(SSR)
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Tab of ANOVA/Effects
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Effect estimates
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STATISTICA TUTORIAL 6
Mean Effect
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STATISTICA TUTORIAL 7
Contour plot
Predicted
response
3D surface
plot
Contour plot