EXPERIMENTAL

DESIGN

Instructor: Lê Ngọc Liễu

Email: lnlieu@hcmiu.edu.vn
Office: A1.706
Content

Chapter 1: Introduction and Basics

Chapter 2: Comparative Experiments

Chapter 3: Factorial Design

Chapter 4: Optimization

Chapter 5: Modeling

Chapter 6: Design of experimental flowchart

 Chapter 3
Screening Experiments
Four general fields applying Design of Experiment

Comparative

Screening

Optimization

Modeling
Screening Experiments

Used when you want to see the effect of a whole range of factors so as to know
which one(s) are most important.

Screening experiments:

Simple design: one factor at a time

Full factorial design: 2k

Half factorial design: 2k-1

Plackett-Burnam design
Simple design

Start with a configuration and vary one factor at a time

Given k factors and the i-th factor having ni levels

The required number of experiments

Example:
Simple design: one factor at a time
Example:

Investigate the effects
Factor 1: enzyme concentration: 0.01; 0.02; 0.03%

of enzymatic treatment
on fruit juice yield
Factor 2: treatment duration: 30, 60, 90, 120 min

Factor 3: treatment temperature: 30, 60 oC

1 2 3 4 5 6 7
Enzyme concentration 0.02 0.02 0.01 0.03 0.03 0.03 0.03
Treatment duration 90 90 90 90 30 60 120
Treatment temperature 30 60 60 60 60 60 60

How to determine the number of factors and number of levels?

Simple design: one factor at a time
Common procedure

Identify a key factor

Make changes to the key factor while trying to hold all other factors constant.

Evaluate the effect

Alter the process (maybe)

Repeat
Simple design: one factor at a time
Principle to be considered in determination of levels:

Each numeric factor should generally have at least 3 levels

There should exist a peak or plateau in the trend of change

Statistical analysis should be applied to determine the peak/ plateau

Control sample should be included

 peak
Simple design: one factor at a time
90 90 a 90 a
80 80 b 80 b
70 70 c 70 c c
60 60 60

Yield (%)
Yield (%)

Yield (%)
50 50 50
40 40 40
30 30 30
20
20 20
10
10 10
0
0 0 30 60 90 120
30 60 30 60 90
Treatment duration (min)
Treatment duration (min) Treatment duration (min)

plateau
90 90 a
a 80 b
80 a
70 b 70 c c
60 60

Yield (%)
d
Yield (%)

50 50
40 40
30 30
20 20
10 10
0 0
30 60 90 0 30 60 90 120
Treatment duration (min) Treatment duration (min)
Simple design: one factor at a time
Disadvantages

Require more runs for the same precision in effect estimation

Cannot estimate interactions

Can miss optimal settings of factors

1 2 3 4 5 6 7
Enzyme concentration 0.02 0.02 0.01 0.03 0.03 0.03 0.03
Treatment duration 90 90 90 90 30 60 120
Treatment temperature 30 60 60 60 60 60 60
Full factorial design

Use all possible combinations at all levels of all factors

Given k factors and the i-th factor having ni levels

The required number of experiments

Example:
Fractional factorial design

When full factorial design results in a huge number of experiments, it

may be not possible to run all

Use subsets of levels of factors and the possible combinations of these

Given k factors and the i-th factor having ni levels; and selected subsets of
levels mi ≤ ni.

The required number of experiments

Example:
Comparation of experiment runs
Main effect and interaction

The main effect of a factor is defined to be the change in response

produced by a change in the level of a factor.

In some experiments we may find that the difference in response

between the levels of one factor is not the same at all levels of the other
factor. When this occurs, there is an interaction between the factors.
Main effect and interaction

Graphs are frequently useful in interpreting significant interactions.

When an interaction is large, the main effects have little practical

meaning.

A significant interaction will often mask the significance of main effects.

Advantages of Factorials

They are more efficient than one-factor-at-a-time experiments.

A factorial design is necessary when interactions may be present to

avoid misleading conclusions.

Factorial designs allow the effects of a factor to be estimated at several

levels of the other factors, yielding conclusions that are valid over a
range of experimental conditions.
Full factorial design

Easy design to create. Each factor is tested at each condition of the factor

Popcorn microwave making example:

2 brands x 6 power settings x 3 time settings = 36 trials

Results analyzed with a linear model

Cost: resources, time, materials. What if you can’t afford 36 trials? What if
you only have 16 bags of popcorn?
2k Factorial Designs

Test each of k factors at 2 levels

Begin by experimenting at the minimum and maximum level of a factor

 two levels

A total of 2k experiments are required

Advantages • Less experiment runs

• Help to identify important factors (screening)

Disadvantages • Cannot identify nonlinear effects

• Follow-up with additional sampling on important factors

(augment design)
 Standard 23 Sign Table

Randomization Run A B C Response

1 - - -
2 - - +
3 - + -
4 - + +
5 + - -
6 + - +
7 + + -
8 + + +
Standard 23 Sign Table (with result)

Run Temp (oC) Time (min) Ingredient Yield (%)

1 200 1 1 65.3
2 200 1 2 81.3
3 200 2 1 53.3
4 200 2 2 69.9
5 250 1 1 61.8
6 250 1 2 77.4
7 250 2 1 73.9
8 250 2 2 89.9
2k Factorial Designs
Principle to be considered

Be aggressive in setting factor levels, but not exceed the extreme

Always randomize run order

2k Factorial Designs
Example: popcorn microwave making

Be aggressive in setting factor levels, but not exceed the extreme (burn
popcorn)
2k Factorial Designs
Example: popcorn microwave making

Always randomize run order

2k-p Fractional Factorial Designs

To do a full 2k factorial experiment, you must do at least 2k runs

• Testing 4 factors costs twice as much as testing 3 factors

When the number of factors is large, a full factorial design requires a

large number of experiments

In that case fractional factorial design can be used

• Require fewer experiments, e.g., 2k-1 requires half of the experiments as

a full factorial design
2k-p Fractional Factorial Designs

Condition combinations are chosen to provide sufficient information to

determine the factor effect

Key point, what subset of factor combinations?

• Pick the wrong set and you’re likely to miss interactions

• DoE software can help

2k-p Fractional Factorial Designs

Confounding
• with fractional factorial design some of the effects can not be determined

• only combined effects of several factors can be computed

A fractional factorial design is not unique

Design resolution

• The resolution of a design is measured by the order of effects that are

aliased (or confounded)

• A design of higher resolution is considered a better design, but require

more runs
Plackett-Burman design

This design screens out unimportant factors (noise), which means that
you avoid collecting large amounts of data on relatively unimportant
factors.

Number of factor

• Only be used for experiments that are multiples of 4 with 8 as the

starting point (N = 8, 12, 16, 20, 24, 28, 32, 36)

• A minimum of 4n experiments is needed for estimating main effects

for 4n-1 factors

For example, 4, 5, 6, or 7 factors would require at least 8 experimental

runs, 8, 9, 10, or 11 would require at least 12 runs, and so on.
Plackett-Burman design

Advantage

Sort out which factors to concentrate on, greatly reducing the amount of
data you have to collect.

• For example, with 15 factors in your design, 20 data points needed in

a Plackett-Burman. A full factorial design would require over a
thousand times that amount (32,768 data points).
Plackett-Burman design

It is particularly helpful to use Plackett-Burman design:

In screening

When neglecting higher order interactions is possible

In two-level multi-factor experiments

When there are more than four factors (if there are between two to four
variables, a full factorial can be performed)

To economically detect large main effects

For N = 12, 20, 24, 28 and 36 (where N = the number of experiments)
Plackett-Burman design

Disadvantage

They do not verify if the effect of one factor depends on another factor.

If you run the smallest design you can, it does not follow that enough data
has been collected to know what those effects are precisely.

Plackett-Burman should be used as a starting point for further

experiments. Once the important factors have been identified, a
full factorial or fractional design should be run to study those
factors more.
2k-1 Fractional Factorial
Design Example

Case study 3.1

Chang, Siu Hua, Tjoon Tow Teng, and Norli Ismail.
"Screening of factors influencing Cu (II) extraction
by soybean oil-based organic solvents using
fractional factorial design." Journal of environmental
management 92.10 (2011): 2580-2585
Analysis procedure for a factorial design

Estimate factor effects

Statistical testing (ANOVA) + Formulate model

Refine the model

Analyze residuals (graphical)

Interpret results
Estimate factor effects
Estimate factor effects
Estimate factor effects
Statistical testing (ANOVA) + Formulate model
Regression analysis

High-order interactions are neglected

Regression model for %E (y)

Refine model

Reduced model for %E (in coded units)

Reduced model for %E in uncoded units

%E = -239.4 + 2.823 B + 74.03 E - 0.6160 BE

Analyze residuals (graphical)
 Total number of experiments: 25 = 32

Full factorial Table 1: Five Factor Analyses with Two Levels (Full Factorial Design)
A B C D E Y
Total number of experiments: 12
vs. -1
1
-1
-1
-1
-1
-1
-1
-1
-1
75.87
76.14
-1 1 -1 -1 -1 109.95
Plackett- 1 1 -1 -1 -1 109.55
Table 2: Five Factor Analysis with Two Levels (Plackett-Burman Design)
A B C D E Y
-1 -1 1 -1 -1 80.17
Burman 1
-1
-1
1
1
1
-1
-1
-1
-1
80.3
114.07
1 -1 1
-1
-1 -1
-1
75.67
1 1 1 102.4
1 1 1 -1 -1 114.05
-1 -1 -1 1 -1 68.77 -1 1 1 -1 1 113.71
1 -1 -1 1 -1 68.63 1 -1 1 1 -1 72.95
5 factors, 2 levels -1 1 -1 1 -1 102.41
1 1 -1 1 1 102.32
1 1 -1 1 -1 102.27
-1 -1 1 1 -1 72.95 1 1 1 -1 1 113.85
1 -1 1 1 -1 72.68 -1 1 1 1 -1 106.51
-1 1 1 1 -1 106.98
-1 -1 1 1 1 72.66
1 1 1 1 -1 106.65
-1 -1 -1 -1 1 75.79 -1 -1 -1 1 1 68.62
1 -1 -1 -1 1 75.71 1 -1 -1 -1 1 75.54
-1 1 -1 -1 1 110.08
1 1 -1 -1 1 110.04 -1 1 -1 -1 -1 109.28
-1 -1 1 -1 1 80.49 -1 -1 -1 -1 -1 75.69
1 -1 1 -1 1 80.86
-1 1 1 -1 1 113.49
1 1 1 -1 1 114.06
-1 -1 -1 1 1 68.22
1 -1 -1 1 1 68.6
-1 1 -1 1 1 102.5
1 1 -1 1 1 102.3
-1 -1 1 1 1 73.03
1 -1 1 1 1 73.3
-1 1 1 1 1 106.08
1 1 1 1 1 106.7
Full factorial vs. Plackett-Burman

High-order interactions: only consider second-order

Full factorial vs. Plackett-Burman
Full factorial vs. Plackett-Burman

Comparison of Results
Full Factorial Design Plackett-Burman Design
Number of experiments 32 12
Significant factors B, C, D B, C, D
Significant levels B: +1, C: +1, D: -1 B: +1, C: +1, D: -1
Significant interactions (B, C) and (A, E)* Non-detectable
Optimized value of Y 114.13 113.66
*If considered at p < 0.1
Half fractional factorial design – extra example
Half factorial design was used to screen the effect of 5 factors on the response to obtain the following table. Use
Minitab to compute the regression equation of the response. Provide the effect order (Pareto chart) of all factors
and their interaction.

StdOrder RunOrder CenterPt Blocks A B C D E Response

7 1 1 1 2 80 80 30 100 43.02
5 2 1 1 2 20 80 30 10 5.62
13 3 1 1 2 20 80 300 100 31.88
2 4 1 1 6 20 30 30 10 16.7
17 5 0 1 4 50 55 165 55 32.38
3 6 1 1 2 80 30 30 10 18.15
16 7 1 1 6 80 80 300 100 48.88
10 8 1 1 6 20 30 300 100 29.02
15 9 1 1 2 80 80 300 10 9.4
19 10 0 1 4 50 55 165 55 31.52
12 11 1 1 6 80 30 300 10 17.29
14 12 1 1 6 20 80 300 10 13.52
8 13 1 1 6 80 80 30 10 14.4
18 14 0 1 4 50 55 165 55 33.33
11 15 1 1 2 80 30 300 100 41.73
6 16 1 1 6 20 80 30 100 38.73
4 17 1 1 6 80 30 30 100 24.59
9 18 1 1 2 20 30 300 10 17.28
1 19 1 1 2 20 30 30 100 16.3
Half fractional factorial design – extra example