Section 1
INTRODUCTION
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB  1.1 Revised 3/10/2000
WHAT IS DESIGN OF EXPERIMENTS (DOE)? DOE is a strategic process, with supporting methods and tools, for guiding the  planning  execution  analysis of results  application of results of experimental or developmental programs.
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB  1.2 Revised 3/10/2000
BENEFITS OF DOE
Highest leverage quality tool available  use to design quality in up front Reduces product/process development cycle time Most efficient strategy for gaining process understanding Develops true causeandeffect relationships Provides solution to current problem plus
information for solving future problems
An objective, factbased system for decision making, complete with quantitative measures of uncertainty
SOE/MTB  1.3 Revised 3/10/2000
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
WHERE CAN DOE BE APPLIED?
DOE is useful in every stage of product life cycle
– Product and Process Development – Process ScaleUp, Operations Startup, Customer Verification – Process Control, Product and Process Improvement
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB  1.4 Revised 3/10/2000
APPLICATIONS IN PRODUCT AND PROCESS DEVELOPMENT Define and translate customer needs Design robust products Design robust processes Reduce time to commercialization Develop test methods Define operating procedures Enhance business integration of R&D with Operations
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB  1.5 Revised 3/10/2000
APPLICATIONS IN SCALEUP, STARTUP AND CUSTOMER VERIFICATION
Reduce time to process qualification Identify key process variables Determine product specifications Design product field tests Develop standard operating conditions and standard operating procedures
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB  1.6 Revised 3/10/2000
APPLICATIONS IN PROCESS CONTROL Develop process models Calibrate process control knobs Adjust to changing customer needs Troubleshoot process problems Develop sampling protocols
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB  1.7 Revised 3/10/2000
1.APPLICATIONS IN PRODUCT AND PROCESS IMPROVEMENT Reduce product variability Improve firstpass firstquality yield Increase capacity Reduce transition time Make process more robust Improve test methods
DuPont Quality Management and Technology © 2000 E. I.8 Revised 3/10/2000
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SOE/MTB .
du Pont de Nemours and Company SOE/MTB . widelyapplicable tools for designing and analyzing experiments Handson experience at using these tools Some sense of when and where to seek expert help
DuPont Quality Management and Technology © 2000 E.WHAT YOU SHOULD GET OUT OF SOE An appreciation of the basic underlying concepts of DOE A general strategy for approaching experimentation A set of efficient.9 Revised 3/10/2000
.1. I.
du Pont de Nemours and Company
SOE/ECHIP .1 Revised 3/10/2000
. I.Section 2
WORKSHOP 1
DuPont Quality Management and Technology © 2000 E.2.
ABBREV.5.2 Revised 3/10/2000
.15*T . Prior work has indicated that COLOR may be affected by the following variables.0*A
DuPont Quality Management and Technology © 2000 E. C T A VARIABLE NAME Catalyst Concentration Reactor Temperature Additive Amount EXP. du Pont de Nemours and Company SOE/ECHIP . RANGE LOW HIGH 1.2.5 + 100*C + 0. I.8 130 190 1 5 UNITS % deg C kg
Also from prior work. One major problem remains: the COLOR (yellowness) has often been unacceptable in experimental production to date.0 1. The COLOR value should be made as low as possible. it is known that MODULUS can be predicted by the following equation over the experimental range of interest:
MODULUS = 69.WORKSHOP 1 PROBLEM
A new polymer is being readied for a plant process.
du Pont de Nemours and Company SOE/ECHIP .WORKSHOP 1 PROBLEM
Your problem is: 1. To demonstrate an approximate set of conditions to obtain low COLOR together with low MODULUS.3 Revised 3/10/2000
. and 2. COLOR. Your boss’s best guess of a good place to start is: CATALYST = 1. I.2.25 % TEMPERATURE = 137 deg C ADDITIVE = 3 kg
DuPont Quality Management and Technology © 2000 E. To support your conclusion with a description of the effects of the factors on the response.
Cata Temp Addi Runs Method/Comments Rec. du Pont de Nemours and Company SOE/ECHIP .4 Revised 3/10/2000
. I. Settings Results Effects on Color
1 2 3 4 5 6 7 8 9 10
DuPont Quality Management and Technology © 2000 E.2.WORKSHOP 1 TEAM REPORTS
Team
# of Cata Temp Addi Color Mod.
2.5 Revised 3/10/2000
. Cata Temp Addi
# of Runs Method/Comments
11 12 13 14 15 16 17 18 19 20
DuPont Quality Management and Technology © 2000 E. I. Settings Results Effects on Color
Team Cata Temp Addi Color Mod. du Pont de Nemours and Company SOE/ECHIP .WORKSHOP 1 TEAM REPORTS
Rec.
I.6 Revised 3/10/2000
.WORKSHOP 1:
Concepts Introduced
Experimental Variability Is a Fact of Life Properties Can Be Represented As Functions of Control Variables Geometry of Experimental Region Contour Plots Interaction Multiple Responses
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SOE/ECHIP .
Section 3
FOUNDATIONS OF THE STRATEGY
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SOE/ECHIP . I.3.1 Revised 7/02/2000
.
UNDERLYING PRINCIPLES World is multivariate Experimental error is a fact of life Experimentation is a process Multistage approach Statistical strategy The 6 B’s of DOE
DuPont Quality Management and Technology © 2000 E.2 Revised 7/02/2000
.3. I. du Pont de Nemours and Company
SOE/ECHIP .
hold time.g. modulus. synergistic or antagonistic effects Usually. hardness. several responses (outcomes) of interest
e. flow rate. assay. I.e. yield. color. pH. pressure.3 Revised 7/02/2000
. viscosity.WORLD IS MULTIVARIATE
Almost always more than one factor of interest that can be varied
e. screw speed
Interactions often present .g. dyeability
Tradeoffs between responses often necessary
DuPont Quality Management and Technology © 2000 E.3. du Pont de Nemours and Company
SOE/ECHIP .factor effects not additive i. temperature.
3. I.VARIABLES
FACTORS
variables that are deliberately controlled in the experiment
RESPONSES
outcome variables that are measured during the experiment
LURKING VARIABLES
variables that are unidentified or uncontrolled
synonyms
INDEPENDENT VARIABLES PREDICTORS KNOBS PROCESS VARIABLES TREATMENTS DOSES DEPENDENT VARIABLES PROPERTIES CHARACTERISTICS OUTCOMES NOISE UNCONTROLLED VARIABLES
DuPont Quality Management and Technology © 2000 E.4 Revised 7/02/2000
. du Pont de Nemours and Company
SOE/ECHIP .
5 Revised 7/02/2000
.the catchall term used to explain why results are not identical from replicate to replicate 2 types of experimental error:
– systematic or bias error – random error
DuPont Quality Management and Technology © 2000 E.3.EXPERIMENTAL ERROR Experimental error is the “noise” in the system . I. du Pont de Nemours and Company
SOE/ECHIP .
du Pont de Nemours and Company
SOE/ECHIP .6 Revised 7/02/2000
.RANDOM ERROR
0
0
• Unpatterned variability • Unpredictable • Multiple unassignable causes
• Normal error distribution • Standard deviation represents “typical” error
DuPont Quality Management and Technology © 2000 E. I.3.
SYSTEMATIC OR BIAS ERROR
•Patterned variation •May be predictable •Due to single assignable cause
–e. I.7 Revised 7/02/2000
.g. ambient temperature
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SOE/ECHIP . day. shift.3.
du Pont de Nemours and Company
SOE/ECHIP .8 Revised 7/02/2000
.3.DEALING WITH EXPERIMENTAL ERROR
EXPERIMENTAL ERROR
RANDOM ERROR
SYSTEMATIC ERROR Assignable Patterned Blocking Randomization
CAUSE NATURE REMEDY
Unassignable Unpatterned Replication
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feature of all good designs –Pure replication (as above)
DuPont Quality Management and Technology © 2000 E. I.REPLICATION
true relationship true relationship
RESPONSE
random error random error fitted relationship
RESPONSE
average
fitted relationship
average
FACTOR
FACTOR
•Through averaging of replicates the impact of random error is reduced •Two forms of replication
–Hidden replication .9 Revised 7/02/2000
. du Pont de Nemours and Company
SOE/ECHIP .3.
du Pont de Nemours and Company SOE/ECHIP .10 Revised 7/02/2000
.BLOCKING
Used in presence of identifiable source of potential bias (“blocking factor”)
– e. any block effect with that of an experimental factor.3. day.g. I.
DuPont Quality Management and Technology © 2000 E. or confusing. This prevents confounding. raw material lot
Split the experiment up into blocks representing different levels of the blocking factor Keep the blocks balanced with respect to the experimental factors.
11 Revised 7/02/2000
. randomize within blocks May require constrained randomization if some experimental factors hard to change
DuPont Quality Management and Technology © 2000 E.RANDOMIZATION “Insurance” protection against potential unidentified sources of bias Randomize the order of experimental runs If experiment is blocked. I.3. du Pont de Nemours and Company
SOE/ECHIP .
du Pont de Nemours and Company
SOE/ECHIP .12 Revised 7/02/2000
. I.EXPERIMENTATION IS A PROCESS
Gather Information Apply Results Define Objectives no Update Information yes Run Experiment Design Experiment
Go to next stage of experimentation?
Analyze Experiment Perform Confirmation Runs
Interpret Results
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I. du Pont de Nemours and Company
SOE/ECHIP .3.MULTISTAGE APPROACH
SCREENING DESIGNS INTERACTION DESIGNS RESPONSE SURFACE DESIGNS
Evolution of the Experimental Environment
NUMBER OF FACTORS OBJECTIVE COMMON DESIGNS
6 or more 38 26
Identify key factors
Understand factor interactions Full Factorial Fractional Factorial (resolution 5)
Prediction model Optimization BoxBehnken Central Composite Face Center Cube
PlackettBurman Fractional Factorial (resolution 3 or 4)
DuPont Quality Management and Technology © 2000 E.13 Revised 7/02/2000
.
du Pont de Nemours and Company
SOE/ECHIP .14 Revised 7/02/2000
.STATISTICAL STRATEGY VS. I.3. ONEFACTORATATIME
OneFactorAtATime
Levels of X2
Statistical
Levels of X2
Y
Y
X1
X1
DuPont Quality Management and Technology © 2000 E.
15 Revised 7/02/2000
. I. separately for each factor Ignored
STATISTICAL
Vary all factors jointly in balanced bitesized spacefilling design Simple empirical models based on loworder polynomials Recognized and estimated
FITTED MODEL
EXPERIMENTAL ERROR INTERACTIONS
Not considered. keeping all others fixed Curves fitted through data points. du Pont de Nemours and Company
SOE/ECHIP . in multiple small increments. not estimable
Dealt with as appropriate
DuPont Quality Management and Technology © 2000 E.COMPARING THE STRATEGIES
1FACTORATATIME
DESIGN
Vary only 1 factor at time.3.
3. du Pont de Nemours and Company
SOE/ECHIP . and estimate experimental error
Boldness
– Vary experimental factors over wide range – Measure all relevant responses
Balance
– Use balanced designs to maximize efficiency and minimize confounding
Bias Error
– Take countermeasures such as randomization and blocking
Blunders
– Avoid through careful planning and execution
Batting Average
– Improve your odds of success through statistical designs and empirical modeling
DuPont Quality Management and Technology © 2000 E. achieve desired sensitivity. I.16 Revised 7/02/2000
.6 B’S OF DOE
Bite Size
– Just enough runs to meet objectives.
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SOE/ECHIP .1 Revised 3/10/2000
.4.Section 4
FACTORIAL GEOMETRY
DuPont Quality Management and Technology © 2000 E.
2 Revised 3/10/2000
. I. du Pont de Nemours and Company
SOE/ECHIP .4.EVOLUTION OF THE ENVIRONMENT: Intermediate Stage
SCREENING DESIGNS
INTERACTION DESIGNS
RESPONSE SURFACE DESIGNS
Evolution of the Experimental Environment
NUMBER OF FACTORS OBJECTIVE COMMON DESIGNS
6 or more 38 26
Identify key factors
Understand factor interactions Full Factorial Fractional Factorial (resolution 5)
Prediction model Optimization BoxBehnken Central Composite Face Center Cube
PlackettBurman Fractional Factorial (resolution 3 or 4)
DuPont Quality Management and Technology © 2000 E.
I.4.TWOLEVEL FACTORIAL DESIGNS
2k Distinct Runs Easy to Plan and Analyze Usable for Either Continuous or Discrete Factors with Two Levels Uniformly Spread Through Factor Space Permit Estimation of Both Main Factor Effects and Interaction Effects
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/ECHIP .3 Revised 3/10/2000
.
LO. LO. X2. HI)
(HI. LO) (X1. HI. I.23 FACTORIAL DESIGN
(LO.4. du Pont de Nemours and Company
SOE/ECHIP . LO . X3) = (LO. LO)
X2 X1
(HI. HI) (HI. HI. HI. LO)
DuPont Quality Management and Technology © 2000 E. HI)
(LO.4 Revised 3/10/2000
. HI. HI)
X3
(HI. LO) (LO. LO.
du Pont de Nemours and Company
SOE/ECHIP .8 1.0 1.0
190 190 130 190 130 190 130 130
5 1 5 5 1 1 5 1
72 48 37 48 36 74 62 61
114 54 105 34 125 134 25 45
DuPont Quality Management and Technology © 2000 E.0 1.8 1.8 1.8 1.5 Revised 3/10/2000
.3 FACTOR 2 LEVEL FULLFACTORIAL Experiment Data
CATALYST TEMPERATURE ADDITIVE COLOR MODULUS
1.0 1. I.4.
I.4.6 Revised 3/10/2000
. du Pont de Nemours and Company
7 4 36 X2 (Temperature)
SOE/ECHIP .23 FACTORIAL DESIGN with Workshop 1 COLOR Data
48 62 37 X3 (Additive) 72
48 61 X1 (Catalyst)
DuPont Quality Management and Technology © 2000 E.
EFFECT = YHIGH . Let YHIGH = average of values on HIGH plane.7 Revised 3/10/2000
. du Pont de Nemours and Company SOE/ECHIP .4. I. Let YLOW = average of values on LOW plane.YLOW
DuPont Quality Management and Technology © 2000 E.WHAT IS AN EFFECT ? An effect is the difference in the averages of two groups of observations.
du Pont de Nemours and Company
48 + 62 + 48 + 61 4
=
24 + (25) + 26 + (25) = 0 4
SOE/ECHIP .8 Revised 3/10/2000
. I.4.SAMPLE CALCULATION: EFFECT OF X1
48 62
25 24
72 37 X3 (Additive)
48 61
25
26
74 36 X2 (Temperature)
X1 (Catalyst)
72 + 37 + 74 + 36 4
DuPont Quality Management and Technology © 2000 E.
SAMPLE CALCULATION: EFFECT OF X2
35
48
14
72 37 X3 (Additive)
62
13
48 61 X1 (Catalyst)
74
38
36
X2 (Temperature)
48 + 72 + 48 + 74 4
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
62 + 37 + 61 + 36 4
=
14 + 35 + (13) + 38 = 11.5 4
SOE/ECHIP .4.9 Revised 3/10/2000
. I.
4. I. du Pont de Nemours and Company
74 36 X2 (Temperature)
48 + 74 + 61 + 36 4
=
0 + (2) + 1 + 1 = 0 4
SOE/ECHIP .10 Revised 3/10/2000
.SAMPLE CALCULATION: EFFECT OF X3
48 62
0 1 1
72 37
2
X3 (Additive)
48 61 X1 (Catalyst)
48 + 72 + 62 + 37 4
DuPont Quality Management and Technology © 2000 E.
du Pont de Nemours and Company SOE/ECHIP .4. I.11 Revised 3/10/2000
.ONE FACTOR AT A TIME
X3
No Hidden Replication Not Space Filling
X2 X1
DuPont Quality Management and Technology © 2000 E.
I. du Pont de Nemours and Company
Y
High X2
X1
SOE/ECHIP .12 Revised 3/10/2000
.INTERACTION OF X1 AND X2
INTERACTION
High X2 Y Y Low X2 X1 X1 High X2
Low X2
NO INTERACTION
Low X2 Y High X2 Low X2 X1
DuPont Quality Management and Technology © 2000 E.4.
YC) .YA)] / 2
(YA + YD) (YB + YC)
X1
DuPont Quality Management and Technology © 2000 E.4.(YB . du Pont de Nemours and Company SOE/ECHIP .13 Revised 3/10/2000
. I.INTERACTION GEOMETRY
X1 Effect at High and Low X2 YC YD YB YA X2 = 2 2 X1*X2 Interaction Effect =
[(YD .
YA)] / 2
(YA + YD) (YB + YC)
X1
DuPont Quality Management and Technology © 2000 E.YB) .(YC .14 Revised 3/10/2000
. du Pont de Nemours and Company SOE/ECHIP . I.4.INTERACTION GEOMETRY
X2 Effect at High and Low X1 YC YD YB YA X2 = 2 2 X1*X2 Interaction Effect =
[(YD .
I. du Pont de Nemours and Company
74 36 X2 (Temperature)
48 + 37 + 48 + 36 4
=
25
SOE/ECHIP .4.SAMPLE CALCULATION: X1*X2 INTERACTION EFFECT
48 62 37 X3 (Additive) 72
48 61 X1 (Catalyst)
72 + 74 + 62 + 61 4
DuPont Quality Management and Technology © 2000 E.15 Revised 3/10/2000
.
SAMPLE CALCULATION: X1*X3 INTERACTION EFFECT
48 62 37 X3 (Additive) 72
48 61 X1 (Catalyst)
37 + 72 + 48 + 61 4
DuPont Quality Management and Technology © 2000 E. I.16 Revised 3/10/2000
.4. du Pont de Nemours and Company
74 36 X2 (Temperature)
48 + 62 + 74 + 36 4
=
0.5
SOE/ECHIP .
17 Revised 3/10/2000
. I.4.SAMPLE CALCULATION: X2*X3 INTERACTION EFFECT
48 62 37 X3 (Additive) 72
48 61 X1 (Catalyst)
48 + 72 + 61 + 36 4
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
74 36 X2 (Temperature)
62 + 37 + 48 + 74 4
=
1
SOE/ECHIP .
SAMPLE CALCULATION: X1*X2*X3 INTERACTION EFFECT
48 62 37 X3 (Additive) 72
48 61 X1 (Catalyst)
72 + 62 + 48 + 36 4
DuPont Quality Management and Technology © 2000 E.18 Revised 3/10/2000
. du Pont de Nemours and Company
74 36 X2 (Temperature)
48 + 37 + 74 + 61 4
= 0.5
SOE/ECHIP .4. I.
I.19 Revised 3/10/2000
X1
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
.HALF OF THREEFACTOR INTERACTION SHOWS BALANCE IN ALL FACTOR PAIRS
X3
X1 X3
X2 X2
SOE/ECHIP .4.
20 Revised 3/10/2000
. I.4.USES OF HIGHERORDER INTERACTION GEOMETRY
Blocking
– Basis for Splitting Experiment into Smaller Blocks – Factors Are Balanced Within Blocks
Screening
– Cut Experiment in Half by Using Only One of Blocks – Factors Are Balanced
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SOE/ECHIP .
du Pont de Nemours and Company
.FACTORIAL DESIGNS: Summary
The “Cube” Approach Each Dimension Is a Factor Coding: Low = “” and High = “+” Effects Are Comparisons of “Planes” Hidden Replication Efficiency: All Data Used to Calculate Each Effect HighOrder Interactions
SOE/ECHIP . I.21 Revised 3/10/2000
DuPont Quality Management and Technology © 2000 E.4.
Section 5
FACTORIAL EXAMPLE: Design
Du Pont Quality Management and Technology © 2000 E.1 Revised 5/09/2000
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SOE/MTB . I.5.
2 Revised 5/09/2000
Range 1.FACTORIAL DESIGN EXAMPLE
Design Phase
Follow the example to design a 2level fullfactorial experiment for the workshop 1 problem. I.5.8 130 to 190 1 to 5
. du Pont de Nemours and Company SOE/MTB .0 to 1. Link to Workshop 1 Problem Factors CATALYST CONCENTRATION REACTOR TEMPERATURE AMOUNT OF ADDITIVE Responses COLOR MODULUS Design = FullFactorial with center points Model = Linear + 2 factor interaction terms
Du Pont Quality Management and Technology © 2000 E.
5. I. du Pont de Nemours and Company
SOE/MTB .3 Revised 5/09/2000
.THREEFACTOR CUBE PLOT
X3
X2 X1
Du Pont Quality Management and Technology © 2000 E.
. . . I. . . .5. .TEST FOR CURVATURE
Y
Difference Is Curvature
. . . . . .
Du Pont Quality Management and Technology © 2000 E. .4 Revised 5/09/2000
X
. du Pont de Nemours and Company
0
+
SOE/MTB .
du Pont de Nemours and Company
SOE/MTB . I.5 Revised 5/09/2000
.Du Pont Quality Management and Technology © 2000 E.5.
Du Pont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB . I.6 Revised 5/09/2000
.5.
Du Pont Quality Management and Technology © 2000 E.7 Revised 5/09/2000
. I.5. du Pont de Nemours and Company
SOE/MTB .
5.Du Pont Quality Management and Technology © 2000 E.8 Revised 5/09/2000
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SOE/MTB . I.
I. du Pont de Nemours and Company
SOE/MTB .5.9 Revised 5/09/2000
.Du Pont Quality Management and Technology © 2000 E.
Du Pont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB . I.5.10 Revised 5/09/2000
.
I.11 Revised 5/09/2000
.5. du Pont de Nemours and Company
SOE/MTB .Du Pont Quality Management and Technology © 2000 E.
Du Pont Quality Management and Technology © 2000 E.12 Revised 5/09/2000
. du Pont de Nemours and Company
SOE/MTB . I.5.
Du Pont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB .13 Revised 5/09/2000
. I.5.
5. I.14 Revised 5/09/2000
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SOE/MTB .Du Pont Quality Management and Technology © 2000 E.
du Pont de Nemours and Company
SOE/MTB .15 Revised 5/09/2000
.Du Pont Quality Management and Technology © 2000 E.5. I.
du Pont de Nemours and Company
SOE/MTB .6.1 Revised 1/29/2001
. I.Section 6
ANALYSIS OF TWOLEVEL FACTORIAL DESIGNS
DuPont Quality Management and Technology © 2000 E.
du Pont de Nemours and Company
SOE/MTB .SECTION 6 OVERVIEW How do we know the effects are real ? Computer analysis of the effects How well have we explained the behavior of Y?
DuPont Quality Management and Technology © 2000 E. I.6.2 Revised 1/29/2001
.
HOW DO WE KNOW THE EFFECTS ARE “REAL” ?
If each corner is an average of replicated runs. we can study the repeatability of the effects. 48 Rep. I. du Pont de Nemours and Company
74 36 X2 (Temperature)
SOE/MTB .3 Revised 1/29/2001
. 2 37 X3 (Additive) 72
48 61 X1 (Catalyst)
DuPont Quality Management and Technology © 2000 E. 1 62 Rep.6.
4 Revised 1/29/2001
.6. du Pont de Nemours and Company
SOE/MTB .EXAMINE THE REPLICATES FOR REPEATABILITY (Case 1)
48 62
61 63 46 50
72 37
36 38
73 71
X3 (Additive)
48 61
62 60
49 47
74 36
38 34
75 73
X2 (Temperature)
X1 (Catalyst)
DuPont Quality Management and Technology © 2000 E. I.
EXAMINE THE REPLICATES FOR REPEATABILITY (Case 2)
48 62
19 105 66 30
72 37
57 17
52 92
X3 (Additive)
48 61
24 98
33 63
74 36
54 18
44 104
X2 (Temperature)
X1 (Catalyst)
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB .5 Revised 1/29/2001
.6. I.
du Pont de Nemours and Company SOE/MTB .6.6 Revised 1/29/2001
.THE IMPACT OF EXPERIMENTAL ERROR
Response
Experimental Error Average Relationship
Effect
Low ()
High (+)
Factor
DuPont Quality Management and Technology © 2000 E. I.
. du Pont de Nemours and Company
SOE/MTB .HOW “REAL” ARE THE EFFECTS ?
Must estimate the size of the experimental error.7 Revised 1/29/2001
.
STANDARD DEVIATION: A measure of variability
(Y1. + (Yn .Y)2 + (Y2 .Y)2 + . = s =
DuPont Quality Management and Technology © 2000 E. . Dev.Y)2 n1
Std. I.6.
8
61 63
48
46 50
72
s=1.4 71
s=1.6.4 73
61
62 60
X2 (Temperature)
38 s=2.4
48
s=1.8 34
X1 (Catalyst)
DuPont Quality Management and Technology © 2000 E.4
62
37
36 38
X3 (Additive)
s=1.8 Revised 1/29/2001
. du Pont de Nemours and Company
SOE/MTB . I.4
49 47
74 36
75 s=1.EXAMINE THE REPLICATES FOR REPEATABILITY (Case 1)
s=2.4
73 s=1.
. I. . .1) s22 + .POOLED STANDARD DEVIATION Based on a weighted average of individual squared standard deviations Assumes homogeneous error .1)
DuPont Quality Management and Technology © 2000 E.1) sk2 (n1 .1) + .1) + (n2 . + (nk .1) s12 + (n2 .6.9 Revised 1/29/2001
. du Pont de Nemours and Company
SOE/MTB . .size of experimental error is uniform throughout design region A more reliable estimate of the overall standard deviation
spooled =
(n1 . + (nk .
87
DuPont Quality Management and Technology © 2000 E.10 Revised 1/29/2001
.5
= 1. I. du Pont de Nemours and Company
SOE/MTB .6.COMPUTE THE POOLED STANDARD DEVIATION FOR THE 23 EXAMPLE: (Case 1)
spooled = = =
1*2 + 1*2 + 1*8 + 1*2 + 1*8 + 1*2 + 1*2 + 1*2 1 + 28 8 1 + 1 + 1 + 1 + 1 + 1 + 1
3.
11 Revised 1/29/2001
.INTERPRETING THE STANDARD DEVIATION
4
3
2
1
0
1
2
3
4
SD units
68% 95% 99.6. I.7%
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company SOE/MTB .
6. I. du Pont de Nemours and Company
SOE/MTB .12 Revised 1/29/2001
.DISTRIBUTION OF AVERAGES The distribution of the means of samples of size n is: –More nearly normal
–Narrower
σY = σY
n
DuPont Quality Management and Technology © 2000 E.
13 Revised 1/29/2001
. ERROR = SPooled * SQRT(1/n1 + 1/n2) where n1 = number of observations forming YLOW n2 = number of observations forming YHIGH
DuPont Quality Management and Technology © 2000 E.THE STANDARD ERROR OF A FACTOR EFFECT Represents the PRECISION in an estimated factor effect Can be used to “test” if a factor effect is “statistically significant”
STD. du Pont de Nemours and Company
SOE/MTB . I.6.
95% confidence level
= 2.14 Revised 1/29/2001
. du Pont de Nemours and Company
SOE/MTB .87 * SQRT(1/8 + 1/8) = 0.9
(1.87 is the pooled standard deviation calculated earlier with 8 degrees of freedom)
Tabled tvalue for 8 df.31 (ttable on next page)
DuPont Quality Management and Technology © 2000 E.EXAMPLE CALCULATION OF STANDARD ERROR
Consider the C*T interaction effect The estimated effect = 25 Standard error = 1.6. I.
75 1.12 2.70 2.14 2.11 3.95 2.75 1.71 1.80 2. du Pont de Nemours and Company
SOE/MTB .00 1.09 2.71 1.08 2.07 2.11 2.20 2.94 1.81 1.16 2.57 2.10 2.18 2.82 2.81 2.86 2.31 2.50 3.79 2.72 1.78 1.58 95% 12.96 90% 6.17 3.98 1.92 2.tDISTRIBUTION VALUES FOR TWOSIDED CONFIDENCE INTERVALS
DF 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 30 40 60 120 ∞ 99% 63. I.45 2.31 2.06 2.75 2.35 2.62 2.01 1.78 2.71 3.92 5.60 4.71 1.90 2.13 2.86 1.89 1.23 2.04 2.03 3.05 3.72 1.70 9.68 1.15 Revised 1/29/2001
.01 2.76 1.66 1.92 2.72 1.13 2.83 1.18 2.67 1.36 2.02 2.84 4.36 3.83 2.70 1.66 2.64
DuPont Quality Management and Technology © 2000 E.25 3.26 2.80 1.30 3.85 2.98 2.73 1.6.77 1.88 2.09 2.06 2.73 1.07 2.74 1.70 4.
9 = 28 Compare observed tratio to tabled tvalue: Here tratio > tabled tvalue (28 > 2. du Pont de Nemours and Company
. I.95 (or 95%) confidence level
Note that the C*T interaction is also significant at the 0.SIGNIFICANCE OF AN EFFECT BY SIGNIFICANCE TEST
Consider the C*T interaction effect Observed tratio = (estimated effect)/(std error) = 25.36).6.99 confidence level (28 > 3.16 Revised 1/29/2001
DuPont Quality Management and Technology © 2000 E. How high can we take the confidence level and still be significant? This is related to the Pvalue.0 / 0.
SOE/MTB .31) So the C*T interaction is statistically significant
at the 0.
0000 !
SOE/MTB .(maximum confidence level at which the effect is significant) EXAMPLE: Pvalue of an effect = 0. du Pont de Nemours and Company
.6. usually as a decimal (i.17 Revised 1/29/2001
DuPont Quality Management and Technology © 2000 E. the smaller the Pvalue
Pvalue is commonly displayed by most statistical packages.e.02 So the effect is significant at 98% confidence level For the C*T interaction effect. the Pvalue is 0. I.PVALUE
The Pvalue of an effect is the chance of having observed an effect that large purely due to random
experimental error The larger the effect. between 0 and 1) Pvalue = 1 .
the effect is significant at the specified confidence level Graphical display of uncertainty
DuPont Quality Management and Technology © 2000 E.SIGNIFICANCE OF AN EFFECT BY CONFIDENCE INTERVAL Consider the C*T interaction effect Confidence interval is:
Estimated effect +/.1
Whenever ZERO is not included in the confidence interval.9) = 25 +/.18 Revised 1/29/2001
.(2.31 * 0.9 to 27. du Pont de Nemours and Company SOE/MTB .6.2.1 or 22.(tvalue * standard error)
For this example 95% confidence interval is
25 +/. I.
19 Revised 1/29/2001
.SECTION 6 OVERVIEW How do we know the effects are “real” ?
– Estimate the experimental error (spooled) and the standard error of the effect – Compare the estimated effect with its standard error – ttest or – confidence interval
Computer analysis of the effects How well have we explained the behavior of Y ?
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company SOE/MTB . I.6.
I.20 Revised 1/29/2001
.COMPUTER ANALYSIS OF THE ESTIMATED EFFECTS Two common approaches:
EFFECTS ANALYSIS – Displays each effect and ttest or confidence interval – Follows approach just covered earlier REGRESSION ANALYSIS – Expresses each effect as a slope of a line or coefficient of a model term – Statistically equivalent to an effects analysis
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB .6.
6. I. du Pont de Nemours and Company SOE/MTB .21 Revised 1/29/2001
.STANDARD FACTOR CODING Regression coefficient (slope) = 1/2 effect
Response
Effect
Average Relationship Slope = ∆ / 2
Low (1)
0
High (+1)
Factor
DuPont Quality Management and Technology © 2000 E.
MEANING OF COEFFICIENTS:
Temperature Effect
75
Slope of this line = Regression coefficient = 5.
140
150
160
(0)
170
180
190
(+1)
Temperature
DuPont Quality Management and Technology © 2000 E.75 (using centered/scaled factor settings)
65
C OLOR
5 55
45
35 130
(1)
For this example: Effect = 11. du Pont de Nemours and Company SOE/MTB .5 = expected increase in COLOR from Temperature=130 to 190 (1 to +1) Coefficient = 5.22 Revised 1/29/2001
.6. I.75 = expected increase in COLOR from Temperature=160 (middle) to 190 (0 to +1). Uses orthogonally scaled (1 to +1) factor settings.
56 1. I.4488 0.000 1.00 0.4488 T 122.2500 0.591 0.7500 0.5000 1.5000 0.0000 Coef 54.000 1.4488 0.4488 0.23 Revised 1/29/2001
.11 P 0.0000 0.5000 SE Coef 0.4488 0.000 0.00 27.85 0.0000 11. du Pont de Nemours and Company
SOE/MTB .00 12.294
DuPont Quality Management and Technology © 2000 E.000 0.6.3 FACTOR EXAMPLE (Case 1)
Minitab Effects Table for COLOR Response
Fractional Factorial Fit: COLOR versus Catalyst.0000 12.0000 5. Additive Estimated Effects and Coefficients for COLOR (coded units) Term Constant Catalyst Temperat Additive Catalyst*Temperat Catalyst*Additive Temperat*Additive Effect 0. Temperature.4488 0.7500 0.5000 0.4488 0.0000 25.000 0.81 0.
T: The ratio of the coefficients divided by their standard errors. – If significant.low “plane” averages).uncertainty around the coefficients due to experimental error.6. I.
Expected change in the response per unit change in the term.
Coef: Regression coefficients for the model terms. du Pont de Nemours and Company SOE/MTB .05) imply significance. we are pretty sure that at least the sign (direction) of the relationship is correct
DuPont Quality Management and Technology © 2000 E.24 Revised 1/29/2001
. SE Coef:
Standard error of the coefficient . Effect: Expected change in the response over the entire range of the
term (high “plane” .ITEMS IN THE MINITAB EFFECTS & COEFFICIENTS TABLE Term: Name for model term. P: Probability of observing a coefficient of that magnitude when the true
coefficient is zero. Low values (<. Note carefully the centering and scaling used for these coefficients for interpretation.
6.3 Factor Example (Case 1) Graphical Representation of Factor Effects
Main Effects Plot (data means) for COLOR
1.5
50.0
52.0 Catalyst Temperature Additive
DuPont Quality Management and Technology © 2000 E.0
1. I.5
COLOR
55.0
57. du Pont de Nemours and Company
SOE/MTB .25 Revised 1/29/2001
. 8
0 13
0 19
1
5
60.
du Pont de Nemours and Company
SOE/MTB .8 130 190 1 5
Catalyst
1.3 Factor Example (Case 1) Graphical Representation of the Interactions
Interaction Plot (data means) for COLOR
1 1.8 1
70 55 40
Temperature
190 130
70 55 40
Additive
5 1
70 55 40
DuPont Quality Management and Technology © 2000 E.6. I.26 Revised 1/29/2001
.
8
DuPont Quality Management and Technology © 2000 E.6. I. du Pont de Nemours and Company
SOE/MTB .27 Revised 1/29/2001
.0 Catalyst
1.3 FACTOR EXAMPLE (Case 1)
Minitab Cube Plot for COLOR Response
Cube Plot (data means) for COLOR
48
72
190
48
74
Temperature
62
37
5
Additive 130
61 36
1
1.
6.3 FACTOR EXAMPLE (Case 1)
Pareto Plot of Effects on COLOR
DuPont Quality Management and Technology © 2000 E. I.28 Revised 1/29/2001
. du Pont de Nemours and Company
SOE/MTB .
29 Revised 1/29/2001
. Alpha = . du Pont de Nemours and Company
SOE/MTB . I.3 FACTOR EXAMPLE (Case 1)
Normal Probability Plot for Effects on COLOR
Normal Probability Plot of the Standardized Effects
(response is COLOR.10) A: Catalyst B: Temperat C: Additive
AB
1
B
Normal Score
0
1
0
10
20
Standardized Effect
DuPont Quality Management and Technology © 2000 E.6.
SECTION 6 OVERVIEW How do we know the effects are “real” ? Computer analysis of the effects
– Effects analysis – Regression analysis
How well have we explained the behavior of Y ?
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB . I.30 Revised 1/29/2001
.6.
they can be used to test if additional effects should be accounted for. du Pont de Nemours and Company
SOE/MTB . I.TWO ESTIMATES OF EXPERIMENTAL ERROR
Pure Error Estimate (PE)
– Based on variability among replicate runs under fixed Xsettings – Same as the pooled standard deviation
Lack of Fit Estimate (LOF)
– Based on how well the estimated effects explain the variation in the observed data.31 Revised 1/29/2001
.
When both the PE and LOF estimates are available.
DuPont Quality Management and Technology © 2000 E.6.
AND L. I. #.F. 1 Fit Pure Error Lack of Fit
Available
DuPont Quality Management and Technology © 2000 E. 3. 0. du Pont de Nemours and Company
SOE/MTB . ESTIMATES AVAILABLE ?
Lack of Fit
Not Available
df: 2. 0 df: 2. 0.WHEN ARE P.E.O. 1
Pure Error
Not Available
Key:
df: #. 2.32 Revised 1/29/2001
.6. # df: 2. 0
Available
df: 2.
THE ANALYSIS OF VARIANCE
Statistical technique for evaluating PURE ERROR and LACKOFFIT experimental error Characterizes how well the estimated effects explain the data
DuPont Quality Management and Technology © 2000 E.33 Revised 1/29/2001
.6. du Pont de Nemours and Company
SOE/MTB . I.
34 Revised 1/29/2001
.6. I.ONE FACTOR EXAMPLE
Experiment Worksheet
Row 1 2 3 4 5 6
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
FACTOR 1 1 0 0 1 1
RESPONSE 25 35 60 80 45 55
SOE/MTB .
du Pont de Nemours and Company SOE/MTB .6. I.ONE FACTOR EXAMPLE
Data Graph with Fitted Line
80
Response Y
70
Y = 50 + 10X
60 50 40 30
1
0
1
Factor X
DuPont Quality Management and Technology © 2000 E.35 Revised 1/29/2001
.
682 T 6.ONE FACTOR EXAMPLE
Coefficients and Analysis of Variance Results
The regression equation is RESPONSE = 50. .03 P 0.0 FACTOR Predictor Constant FACTOR S = 19.07 12.0 1900. SE Coef 7.000 10.36 Coef 50.6.0 100.000 .003 0. .0 F 1.36 Revised 1/29/2001
.0 300.0 + 10.906 9.32 1.0 1500.360
Analysis of Variance Source Regression Residual Error Lack of Fit Pure Error Total DF 1 4 1 3 5 SS 400.0 1200. I. du Pont de Nemours and Company
SOE/MTB .0 375.00 P 0.360 0.041
DuPont Quality Management and Technology © 2000 E.0 1200.0 MS 400.
outliers. Estimates SD of experimental error at any fixed set of conditions. I. An appropriate model will have a nonsignificant lack of fit Ftest (high pvalue). du Pont de Nemours and Company
. Might be significant due to missing terms.6. If the model has some significant terms.37 Revised 1/29/2001
Root of MS Pure Error:
DuPont Quality Management and Technology © 2000 E.05). a need for a transformation. the pvalue should be small (<.FURTHER EXPLANATION ON SELECTED COEFFICIENT TABLE ITEMS
Regression
Tests whether any of the model terms explain the behavior of Y (overall test). lack of measurement precision. etc.
Ftest:
Lack
of Fit Ftest:
Square
Pooled standard deviation from replicates. Tests whether model can be improved with existing data.
SOE/MTB .
I.6. du Pont de Nemours and Company SOE/MTB .38 Revised 1/29/2001
.REGRESSION AND LACK OF FIT SIGNIFICANCE
Example 1
14 12 10
Regression pvalue = .Y1
8 6 4 2 0 15 20 25
FACTOR.0000 Lack of fit pvalue = .X
DuPont Quality Management and Technology © 2000 E.5514
RESP.
6. I.5
Regression pvalue = .9641
RESP.5 15 20 25
FACTOR.39 Revised 1/29/2001
.0
4.Y2
5. du Pont de Nemours and Company SOE/MTB .X
DuPont Quality Management and Technology © 2000 E.8833 Lack of fit pvalue = .REGRESSION AND LACK OF FIT SIGNIFICANCE
Example 2
5.
X
DuPont Quality Management and Technology © 2000 E.Y3
7.REGRESSION AND LACK OF FIT SIGNIFICANCE
Example 3
9.5 3.0000
RESP. du Pont de Nemours and Company SOE/MTB .6.5 6. I.5
Regression pvalue = .5 5.40 Revised 1/29/2001
.5 4.5 2.5 15 20 25
FACTOR.8184 Lack of fit pvalue = .5 8.
6 15 20 25
FACTOR. I. du Pont de Nemours and Company SOE/MTB .REGRESSION AND LACK OF FIT SIGNIFICANCE
Example 4
12.X
DuPont Quality Management and Technology © 2000 E.0001 Lack of fit pvalue = .6 8.41 Revised 1/29/2001
.Y4
9.6.6
Regression pvalue = .6 5.6 6.6 11.6 7.0003
RESP.6 4.6 10.6 3.
Case 1
48 62
61 63 46 50
72 37
36 38
73 71
X3 (Additive)
48 61
62 60
49 47
74 36
38 34
75 73
X2 (Temperature)
X1 (Catalyst)
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB . I.42 Revised 1/29/2001
. .BACK TO OUR 3 FACTOR EXAMPLE . .6.
Temperature.4488 0.43 Revised 1/29/2001
.000 1.85 0.4488 0.4488 0.00 27.4488 0.3 FACTOR EXAMPLE (Case 1)
Coefficients Table for COLOR Response
Fractional Factorial Fit: COLOR versus Catalyst.81 0.5000 0.000 0.0000 12.4488 0.6.000 1.000 0.56 1. du Pont de Nemours and Company
SOE/MTB .5000 1.591 0.7500 0.4488 0.294
DuPont Quality Management and Technology © 2000 E.0000 25.0000 0.11 P 0.0000 5. Additive Estimated Effects and Coefficients for COLOR (coded units) Term Constant Catalyst Temperat Additive Catalyst*Temperat Catalyst*Additive Temperat*Additive Effect 0.000 0.5000 SE Coef 0.5000 0.4488 T 122.0000 Coef 54.7500 0.00 12.2500 0.0000 11.00 0. I.
14 3.00 2505.00
Adj SS 529.00 29.00 28.29
0.00 2505.333
F 54. I.500 0.000 3.608
DuPont Quality Management and Technology © 2000 E.000 0.44 Revised 1/29/2001
.000 259.222 1.00
Adj MS 176.00 3063.3 FACTOR EXAMPLE (Case 1)
Analysis of Variance for COLOR Response
Analysis of Variance for COLOR (coded units)
Source Main Effects 2Way Interactions Residual Error Lack of Fit Pure Error Total
DF 3 3 9 1 8 15
Seq SS 529.000
835.00 29.6. du Pont de Nemours and Company
SOE/MTB .72
P 0.00 28.00 1.00 1.
SECTION 6 OVERVIEW How do we know the effects are “real” ? Computer analysis of the effects How well have we explained the behavior of Y ?
– Analysis of variance results –Regression Ftest –Lack of fit test
DuPont Quality Management and Technology © 2000 E. I.45 Revised 1/29/2001
. du Pont de Nemours and Company
SOE/MTB .6.
Section 7
FACTORIAL EXAMPLE: Analysis
Du Pont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB .7.1 Revised 1/29/2001
.
I.2 Revised 1/29/2001
.8 130 to 190 1 to 5 Responses COLOR MODULUS
Design = FullFactorial with center points Model = Linear + twofactor interaction terms
Du Pont Quality Management and Technology © 2000 E.7.0 to 1. du Pont de Nemours and Company
SOE/MTB . We already have response data entered so we’re now ready to analyze the data.FACTORIAL DESIGN EXAMPLE
Analysis Phase
Recall the workshop 1 problem (summarized below) for which we generated a design earlier in ECHIP. Factors CATALYST CONCENTRATION REACTOR TEMPERATURE AMOUNT OF ADDITIVE Range 1.
I.3 Revised 1/29/2001
.7.THREEFACTOR CUBE PLOT OF EXAMPLE WORKSHOP 1 DATA
34 50 51 25 58 57
38 41 80 42 43
72 114 71 36 38 105
Additive
54 60 59
48 49
73 134 74 34 35 125
45
Temperature
Catalyst
KEY: Numbers inside circles = COLOR values Numbers outside circles = MODULUS values
Du Pont Quality Management and Technology © 2000 E. du Pont de Nemours and Company SOE/MTB .
du Pont de Nemours and Company SOE/MTB .7. Replicate of LOF Standard Deviation test
Comments
1 2 3 4 5 6 7 8 9 10
Du Pont Quality Management and Technology © 2000 E. I.Coefficients (circle if significant)
Team
Cata
Temp
Addi
C*T
C*A
T*A
Signif.4 Revised 1/29/2001
.Workshop 1 Revisited
COLOR .
Du Pont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB . I.7.5 Revised 1/29/2001
.
I.6 Revised 1/29/2001
.Du Pont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB .7.
7 Revised 1/29/2001
. du Pont de Nemours and Company
SOE/MTB .Du Pont Quality Management and Technology © 2000 E. I.7.
Du Pont Quality Management and Technology © 2000 E.8 Revised 1/29/2001
. du Pont de Nemours and Company
SOE/MTB .7. I.
9 Revised 1/29/2001
. du Pont de Nemours and Company
SOE/MTB . I.7.Du Pont Quality Management and Technology © 2000 E.
du Pont de Nemours and Company
SOE/MTB . I.7.Du Pont Quality Management and Technology © 2000 E.10 Revised 1/29/2001
.
972 0.04 0.012 308.063 0.125 2.04 0.875 0.063 6.063 1.547
Analysis of Variance for COLOR (coded units) Source Main Effects 2Way Interactions 3Way Interactions Residual Error Curvature Pure Error Total DF 3 3 1 12 1 11 19 Seq SS 770.4500 2.547 0.716 1.4500 1.126 546.716 1.45 697. I.125 Coef 51.19 2093.535 1.01 19.06 565.7.50 Adj MS F 256.063 0.972 0.51 546.01R R denotes an observation with a large standardized residual
Du Pont Quality Management and Technology © 2000 E.06 565.875 0.04 6. ADDITIVE Estimated Effects and Coefficients for COLOR (coded units) Term Constant CATALYST TEMPERAT ADDITIVE CATALYST*TEMPERAT CATALYST*ADDITIVE TEMPERAT*ADDITIVE CATALYST*TEMPERAT*ADDITIVE Effect 0.000 0.5350 13.125 0.013 0.51 546.Fractional Factorial Fit: COLOR versus CATALYST.38 47.000 0.04 0.000
Unusual Observations for COLOR Obs COLOR Fit SE Fit Residual St Resid 4 38.716 1.11 Revised 1/29/2001
.01 19. du Pont de Nemours and Company
.0000 51.063 SE Coef 1.19 18.01 1.002 0.125 22. TEMPERATURE.716 1.000 0.450 0.716 T 33.729 14.773 P 0.50 3446. .
SOE/MTB .66 0.52 0.729 5.972 0.19 18.438 0.716 1.125 13.972 0.81 18.062 11.938 0.716 1. .04 4.19 2093.95 Adj SS 770.62 P 0.
000 0.0 0.0 27524.00 4.000
Analysis of Variance for MODULUS (coded units) Source Main Effects 2Way Interactions 3Way Interactions Residual Error Curvature Pure Error Total . TEMPERATURE.00 0.71 0.71 0.00 P 0. . I.00 0.
Du Pont Quality Management and Technology © 2000 E.000 1.00 0.00 0.00 0.00
F 1E+05 * *
P 0.06455 619.60 40.12 Revised 1/29/2001
.0 0.0 0.000 1.Fractional Factorial Fit: MODULUS versus CATALYST. du Pont de Nemours and Company
DF 3 3 1 12 1 11 19
Seq SS 27524.00 0.06455 0.8
Adj SS 27524.00 0.8 0.80 0.7.8 0.06455 69.50 10.00 SE Coef T 0.0
Adj MS 9174.68 0.000 0.00 0.000 1. ADDITIVE Estimated Effects and Coefficients for MODULUS (coded units) Term Constant CATALYST TEMPERAT ADDITIVE CATALYST*TEMPERAT CATALYST*ADDITIVE TEMPERAT*ADDITIVE CATALYST*TEMPERAT*ADDITIVE Effect 80.07 0.92 0.06455 0.06455 0.0 0.06455 154.000 0.06455 0.8 0. .8 0.00 0.00 0.00 Coef 79.00 0.05774 1378.000 1.00 20.0 0.00 9.00 0.67 0.0 0.00 0.000 * *
SOE/MTB .
du Pont de Nemours and Company
SOE/MTB .13 Revised 1/29/2001
.Du Pont Quality Management and Technology © 2000 E.7. I.
7.14 Revised 1/29/2001
.Du Pont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB .
7.Du Pont Quality Management and Technology © 2000 E.15 Revised 1/29/2001
. I. du Pont de Nemours and Company
SOE/MTB .
7. du Pont de Nemours and Company
SOE/MTB .Du Pont Quality Management and Technology © 2000 E. I.16 Revised 1/29/2001
.
Interaction Plot (data means) for COLOR
CATALYST 1.7.17 Revised 1/29/2001
.8
60
Mean
Centerpoint
50
40
130
190
TEMPERATURE
Du Pont Quality Management and Technology © 2000 E. I.0 70 1. du Pont de Nemours and Company
SOE/MTB .
18 Revised 1/29/2001
.0
1.Main Effects Plot (data means) for MODULUS
Centerpoint
1 .8
13
0
0 19
1
5
120
100
MODULUS
80
60
40 CATALYST TEMPERATURE ADDITIVE
Du Pont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB .7. I.
I.0
1.7.Main Effects Plot (data means) for COLOR
Centerpoint
1 . du Pont de Nemours and Company
SOE/MTB .19 Revised 1/29/2001
.8
13
0
0 19
1
5
60
55
COLOR
50
45
40
CATALYST
TEMPERATURE
ADDITIVE
Du Pont Quality Management and Technology © 2000 E.
7.Du Pont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB .20 Revised 1/29/2001
. I.
Section 8
GOOD EXPERIMENTAL PRACTICE
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/ECHIP  8.1 Revised 3/10/2000
GOOD EXPERIMENTAL PRACTICE
1. Assess the environment 2. Consider the factors 3. Consider the responses 4. Choose an appropriate design 5. Consider strategies for bias error 6. Create the experimental plan 7. Review the plan for operability 8. Avoid blunders 9. Plan for the analysis 10. Report the recommendations
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/ECHIP  8.2 Revised 3/10/2000
1. ASSESS THE ENVIRONMENT Gather basic information Determine current state of understanding Define experimental objectives Define physical environment and constraints Consider experimental error
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/ECHIP  8.3 Revised 3/10/2000
2. CONSIDER THE FACTORS How many and which factors to vary? Which factors to keep fixed, and at what level? Are factors continuous or discrete? How many levels of each factor? How bold in choice of levels?
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/ECHIP  8.4 Revised 3/10/2000
3. CONSIDER THE RESPONSES Consider all responses of potential interest Are responses continuous or discrete? What is effect size of interest? Is measurement error absolute or relative? Anticipate measurement issues
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/ECHIP  8.5 Revised 3/10/2000
4. CHOOSE AN APPROPRIATE DESIGN Identify underlying model Choose appropriate design class Consider desired sensitivity (resolution) in choosing size of design Consider extra runs Practical constraints?
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/ECHIP  8.6 Revised 3/10/2000
NUMBER OF RUNS VS. SENSITIVITY
SOE Rule of Thumb for balanced 2level factorial designs:
n =
2
( ∆/σ )
7 or 8
∆ = smallest size effect worth detecting σ = standard deviation of experimental error ∆ / σ is “signaltonoise ratio” ∆/σ n
0.5 196256
1.0 4964
1.5 2228
2.0 1216
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/ECHIP  8.7 Revised 3/10/2000
5.8 Revised 3/10/2000
. STRATEGIES FOR BIAS ERROR
Consider blocking to protect against bias due to identifiable variables
– e. operator
Use randomization to protect against bias due to unidentified variables Consider possible constraints on randomization. do restricted randomization if necessary Assess randomization. du Pont de Nemours and Company SOE/ECHIP .g. adjust if necessary
DuPont Quality Management and Technology © 2000 E. material batch. time.8. I.
9 Revised 3/10/2000
.8.6. CREATE THE EXPERIMENTAL PLAN Create experimental worksheet. in randomized run order Express factor levels in actual physical units Include blank columns for responses Write detailed protocol with explicit instructions for every step
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/ECHIP . I.
REVIEW PLAN FOR OPERABILITY
Include all relevant parties in review
– Planner – Executor – Lab analyst – Local experts – Statistician
Examine all runs for operability.10 Revised 3/10/2000
. adjust if necessary Consider constraints on experiment. feasibility of schedule
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company SOE/ECHIP .8.7.
11 Revised 3/10/2000
.8. I. du Pont de Nemours and Company
SOE/ECHIP . AVOID BLUNDERS Anticipate problems in advance Emphasize importance of adhering to experimental protocol Avoid shortcuts Understand importance of each run Avoid stopping short Record any deviations from plan
DuPont Quality Management and Technology © 2000 E.8.
I.9. du Pont de Nemours and Company
SOE/ECHIP .12 Revised 3/10/2000
.8. PLAN FOR THE ANALYSIS
Consider analysis issues in advance
– Models – Software – Method of analysis – Organization of data
Plot the data
DuPont Quality Management and Technology © 2000 E.
REPORT RECOMMENDATIONS Relate recommendations to the objective Recognize value of negligible effects Avoid extrapolation Report raw data for credibility Provide direction for future action
DuPont Quality Management and Technology © 2000 E.10.13 Revised 3/10/2000
. du Pont de Nemours and Company
SOE/ECHIP . I.8.
Section 9
SCREENING DESIGNS
DuPont Quality Management and Technology © 2000 E. du Pont de Nemours and Company
SOE/MTB . I.9.1 Revised 9/26/2000
.
EVOLUTION OF THE ENVIRONMENT: Early Stage
SCREENING DESIGNS
INTERACTION DESIGNS RESPONSE SURFACE DESIGNS
Evolution of the Experimental Environment
NUMBER OF FACTORS OBJECTIVE COMMON DESIGNS
6 or more 38 26
Identify key factors
Understand factor interactions Full Factorial Fractional Factorial (resolution 5)
Prediction model Optimization BoxBehnken Central Composite Face Center Cube
PlackettBurman Fractional Factorial (resolution 3 or 4)
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB  9.2 Revised 9/26/2000
CHARACTERISTICS OF SCREENING DESIGNS Number of runs n only a few more than number of factors k Factors considered at two levels each k Use a fraction of the full 2 factorial design Designs balanced (orthogonal) Main factor effects clear of each other Interactions generally not estimable Twoway interactions may be fully or partially confounded with main effects
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company SOE/MTB  9.3 Revised 9/26/2000
CLASSES OF SCREENING DESIGNS
PlackettBurman (PB) designs Fractional Factorial (FF) designs
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SOE/MTB  9.4 Revised 9/26/2000
PLACKETTBURMAN DESIGNS Available in sizes n which are multiples of 4 Can handle up to n1 factors, although recommended maximum is n5 Tables available for commonly used sizes of n=12, 20, 24, 28 For n equal to power of 2 (e.g. 8, 16, 32,...), same as Fractional Factorial designs Twoway interactions partially confounded with each main effect (for n not a power of 2)
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company SOE/MTB  9.5 Revised 9/26/2000
12 RUN PLACKETTBURMAN DESIGN
Trial 1 2 3 4 5 6 7 8 9 10 11 12 X1 + + + + + + X2 + + + + + + X3 + + + + + + X4 + + + + + + X5 + + + + + + X6 + + + + + + X7 + + + + + + X8 + + + + + + X9 + + + + + + X10 + + + + + + X11 + + + + + + each row a cyclic permutation of previous row
last row all minuses
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company SOE/MTB  9.6 Revised 9/26/2000
BALANCE OF 12 RUN PB DESIGN
Illustrate using factors X1 and X2 Rows rearranged according to level of X1 Trial 1 2 4 5 6 10 3 7 8 9 11 12 X1 + + + + + + X2 + + equal number + of + and + + + 
SAME BALANCE TRUE FOR ANY PAIR OF FACTORS (COLUMNS ARE “ORTHOGONAL”)
equal number of + and 
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
SOE/MTB  9.7 Revised 9/26/2000
PARTIAL CONFOUNDING IN 12 RUN PB
Illustration showing partial confounding between X1 and X2*X3 interaction. Rows rearranged according to level of X1. Trial 1 2 4 5 6 10 3 7 8 9 11 12 X1 + + + + + + X2 + + + + + + X3 + + + + + + X2*X3 + 2 +’s 4 ’s + + + + +
not completely balanced
4 +’s 2 ’s
If there is an X2*X3 interaction effect, it will slightly bias the estimate of the X1 effect (as well as all other main effects except X2 and X3).
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company SOE/MTB  9.8 Revised 9/26/2000
I. assign factors to any columns of the design If blocking.9.USING PLACKETTBURMAN DESIGNS If using tabled design. du Pont de Nemours and Company
SOE/MTB .9 Revised 9/26/2000
. use additional column(s) to define blocks Save at least 4 columns for estimating experimental error Assess sensitivity of design .if inadequate:
– Use larger design – Add reflected design
DuPont Quality Management and Technology © 2000 E.
9. I. 2 FF design is a 1/2p fraction of a full 2k factorial design 16 and 32 run designs most useful for screening Confounding between any two effects is either total or absent Degree of confounding determined by Resolution of design
DuPont Quality Management and Technology © 2000 E.FRACTIONAL FACTORIAL DESIGNS Available design sizes in powers of 2 kp For k factors. du Pont de Nemours and Company SOE/MTB .10 Revised 9/26/2000
.
These are called the defining relations of the fractional factorial design. or the negative of.CONSTRUCTING FF DESIGNS
TO CONSTRUCT 2kp DESIGN.
DuPont Quality Management and Technology © 2000 E. I. Construct a full factorial design in kp of the factors. tables are available of good choices for the defining relations which will result in the highest possible resolution design. a judiciously selected interaction among some of the first kp factors.9. 2. Define each of the p additional factors as equal to. For given values of k and p. WHERE k = NUMBER OF FACTORS: 1. du Pont de Nemours and Company
SOE/MTB .11 Revised 9/26/2000
.
DENOTE FACTORS BY 1. Define factor 4 equal to 123 interaction 1 + + + + 2 + + + + 3 + + + + 4=123 + + + + Defining Relation 4=123 induces additional relations: 1=234 12=34 2=134 13=24 3=124 14=23
1234=I (I =column of all +)
NOTE THAT EFFECTS ARE CONFOUNDED IN PAIRS: main effects with 3way 2way with 2way 4way with mean THIS IS A RESOLUTION 4 DESIGN
DuPont Quality Management and Technology © 2000 E. 2.FOR SIMPLICITY. 3 2. 4 1.12 Revised 9/26/2000
. I.9. 2.EXAMPLE 1: CONSTRUCTING A 241 DESIGN
4 FACTORS . 3. Write down full factorial 23 design in factors 1. du Pont de Nemours and Company
SOE/MTB .
3 2. Defining relations: 4 =12 . 2. du Pont de Nemours and Company
SOE/MTB . 4. 5 1. 3. Write down full factorial 23 design in factors 1. 5=13 1 + + + + 2 + + + + 3 + + + + 4=12 + + + + 5=13 + + + + Defining Relations induce additional relations: 1=24=35=12345 3=15=245=1234 5=13=234=1245 25=34=123=145 2=14=345=1235 4=12=235=1345 23=45=134=125 I=124=135=2345
NOTE THAT EFFECTS ARE NOW CONFOUNDED IN GROUPS OF 4 Each main effect is now confounded with a 2way interaction THIS IS A RESOLUTION 3 DESIGN
DuPont Quality Management and Technology © 2000 E.9. I. 2.13 Revised 9/26/2000
.EXAMPLE 2: CONSTRUCTING A 252 DESIGN
5 FACTORS .1.
I. However. In particular. then the effects may be confounded.9. Two effects of order a and b are unconfounded if a+b < R.14 Revised 9/26/2000
. du Pont de Nemours and Company
SOE/MTB .
RESOLUTION 3 PROPERTIES OF DESIGN Main effects clear of each other but confounded with some 2way interactions Main effects clear of each other and of 2way interactions but 2way interactions confounded with each other Main effects and 2way interactions all clear of each other
4
5 or more
DuPont Quality Management and Technology © 2000 E. a main effect is unconfounded with any effects of order less than R1 but may be confounded with an effect of order equal to R1. if a+b ≥ R.RESOLUTION OF A DESIGN
Let R denote resolution of design.
I.AVAILABLE DESIGN SIZES
# OF FACTORS 5 6 7 8 9 10 11 12 FRACTIONAL FACTORIAL R=3 R=4 R=5 8 8 8 16 16 16 16 16 16 16 16 16 32 32 32 32 16 32 64 64 128 128 128 256 PLACKETTBURMAN MIN ≥ 5 DF ERROR 8 8 8 12 12 12 12 16 12 12 16 16 16 16 20 20
Note: All designs listed assuming no replicates and no center points
DuPont Quality Management and Technology © 2000 E.15 Revised 9/26/2000
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I. du Pont de Nemours and Company
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.Section 10
SCREENING EXAMPLE
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double TEMPERATURE TEMP 200° to 250° F MOISTURE MOIST 20% to 80% Response Abbreviation Expected Range PRODUCT HARDNESS Hardness 10 to 200 (Gauge) Design = PlackettBurman Model = Main Effects only Special Notes: In the past daytoday differences with this process have been observed. Factors Abbreviation Settings TENSION CONTROL TENS manual.
DuPont Quality Management & Technology
© 2000 E. automatic MACHINE MACH #1. A preliminary standard deviation estimate of 13 for hardness has been obtained. Detecting changes in hardness of at least 30 units is of interest.2
Revised 9/26/2000
.Screening Design Example
This example is a 2level screening experiment for a product called GLOOP. #2 THROUGHPUT TPUT 10 to 20 gal/min MIXING MIX single. du Pont de Nemours and Company
SOE/MTB 10. Thus. I. this study really involves 7 factors including the blocking variable (DAY). Since we can only make 8 product items per day we would also like to block this design on day.
du Pont de Nemours and Company
SOE/MTB 10.3
Revised 9/26/2000
.2 ⇒ 10 n≥ 30/13 n ≥ 10
2
The smallest PlackettBurman design for n ≥ 10 is the 12 run design The smallest FractionalFactorial design for n ≥ 10 is the 16 run design
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© 2000 E.What Design Size Is Needed?
Using our sample size formula we need at least:
7 = 9. I.
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09 8.055 0. I.592 3.050
Analysis of Variance for Hardness (coded units) Source Main Effects Residual Error Total .3 16586.00 SE Coef 3. .78 P 0.Fractional Factorial Fit: Hardness versus TENS..592 3.592 3.8 F 14.69 3.17 0.25
Revised 9/26/2000
.00 Coef 70.385 0.67 7.7 619.67 61.67 19.001 0.67 13.33 26.58 0.33 0.23 2.592 T 19.592 3.73 P 0. .49 0.0 154.83 9.00 20. DF 7 4 11 Seq SS 15966.010
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© 2000 E. .97 2. du Pont de Nemours and Company
SOE/MTB 10.828 0.931 0.592 3.00 0.0 Adj SS 15966. Estimated Effects and Coefficients for Hardness (coded units) Term Constant TENS MACH TPUT MIX TEMP MOIST DAY Effect 1.33 30.3 Adj MS 2281.50 10.592 3.7 619.000 0.021 0.83 3. MACH.67 0..592 3.
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.Thought Questions
What
would happen if you analyzed this data ignoring the day effect?
Can
we get any information on interactions among the significant effects with this data?
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© 2000 E. du Pont de Nemours and Company
SOE/MTB 10.
I.11.Section 11
WORKSHOP 2: Glyxel Screening
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SOE/MTB .1 Revised 5/09/2000
.
2 Revised 5/09/2000
FACTORS
HIGH LIMIT 800 8 3.valid range approximately 03 % goal = minimize (a maximum of 1% is desirable) LOW LIMIT 4 0. RESPONSES Bend Resistance (BR) .2
UNITS kg/hr % % impurity % psi °C °C °C l/min
Throughput (TP) 200 Additive A Concentration (AC) Additive A Impurity (AI) Catalyst Amount (CA) 0.see description
DuPont Quality Management and Technology © 2000 E.3 150 150 180 10 10 160 10 25 2 blocks needed 190 15 20 °C °C week
SOE/MTB . du Pont de Nemours and Company
. I.7 0.1 Reactor Pressure (RP) 100 Dryer Temperature (DT) 120 Extruder Temperature (ET) Quench Water Temperature (QT) Quench Water Flow Rate (QF) Press Temperature (PT) 140 Storage Temperature (ST) Block (BL) .Problem Description
Use a screening design to determine which of the following twelve factors are the most important in their effects on the two observed responses.valid range approximately 5080 psi goal = target to 68 (acceptable range is 6571) Area Shrinkage (AS) .11.Workshop 2 .
It is expected that at least 500 kg/hr will be needed for acceptable profitability. since we have 20 lots to choose from that span the range of impurity levels listed.Background Information . you may experiment with impurity level and treat it as a continuous variable. From our supplier we receive an an accurate estimate of impurity level through a Certificate Of Analysis for each lot.71 psi.
DuPont Quality Management and Technology © 2000 E. target of 68) Gives a proper balance between enduse strength and customer processing needs. lower is better) Low shrinkage is required to maintain dimensional stability through customers’ processing.Workshop 2 . Impurity levels are dictated by the lot number. Area Shrinkage (AS) (1. property goals should be met with the highest possible throughput (TP).0% maximum. Two critical property goals must be met. Preliminary R&D work has indicated two process variables likely to aid in meeting bending resistance and area shrinkage goals are reactor pressure (RP) and extruder temperature (ET).3 Revised 5/09/2000
. However.11. quench water temperature (QT) and quench water flow rate (QF) have been suggested as potentially affecting either bending resistance or area shrinkage. Impurity levels of this additive (AI) are also believed to affect area shrinkage. Two other variables. There is also a potential market in the military aeronautic and automotive industries. du Pont de Nemours and Company SOE/MTB . will be produced and sold in sheet form.(acceptable range 65 .
Below are brief variable descriptions and key learnings from early R&D work. The product.I
Your R&D team has been assigned to develop a new product for a critical aerospace use. I. First. called Glyxel. Bend Resistance (BR) . Additive A concentration (AC) is suspected to be important for obtaining low area shrinkage. to meet the expected market demand.
Since our catalyst is expensive.11.Background Information . the actual temperature can vary from 140 to 160 deg C.Workshop 2 .1 deg) available for experimental use. in operation. Since it is not possible to complete our 12factor screening design in one week. it is fed into presses for final shaping. Hopefully. quench water would be supplied from a well with an average yearly temperature range from 10 to 15 deg C. your team can better understand how typical quench water temperature variation will affect the process. Another related variable that may enhance quenching is quench water flow rate (QF). I. Dryer temperature (DT) may influence final product properties as well. we would like to test this claim and.II
It is expected that. remove this potential source of variation by blocking (BL) the experiment. a lower level of CA is desirable if property goals can be satisfied. it is only possible to experiment with about 12 run combinations in a week. more importantly. Materials exiting the reactor are fed into a dryer to remove moisture prior to extrusion. due to presstopress differences and temperature control. The catalyst has been thought to enhance molecular structure development.4 Revised 5/09/2000
. Lastly.
DuPont Quality Management and Technology © 2000 E. it is stored for up to two weeks in a warehouse until shipped. High storage temperature (ST) may be related to product property deterioration. Once the product is formed into sheets. However. However. du Pont de Nemours and Company SOE/MTB . you have a temperature controlled water supply (+/. Because a knowledgeable technician has suggested product properties vary from week to week. due to the complicated nature of this process and time required to make process and recipe changes. After our customer receives our product in sheet form. Your R&D team has acquired a similar press for the duration of the experimental program. The press design temperature (PT) is 150 deg C. you will need to run it over two weeks or blocks.
Note.Workshop 2 .5 psi and 0. Assuming we are interested in detecting effects (least important difference) of at least 3.0 psi for BR and 0.BL responses => BR.. will our proposed screening design will have adequate sensitivity? Type BR and AS as the names of two empty columns in the worksheet.
SOE/MTB . This will be a 20run design (with zero replicates). Fill in your team results on the appropriate row of the team report spreadsheets.. Make sure you define factors and responses by the 2letter abbreviations (factors =>TP. AS).5 Revised 5/09/2000
DuPont Quality Management and Technology © 2000 E.11.2 % for AS. As this would only have 3 degrees of freedom to estimate experimental error and should be treated as a resolution 3 fractionalfactorial design (which are more complex to deal with). . . we will pick up here in the next workshop where we will follow up with a response surface design to optimize this process. I. Which factors have significant effects on product properties? What was the experimental error from your results? Perhaps the most important question is: What factors have you selected to be included in further process optimization work? You may identify up to 5 factors to carry forward to the next design stage. The smallest PlackettBurman design which could handle 12 factors is the 16 run design which is actually a fractionalfactorial design. Be prepared to answer the following questions and report your teams results (see team report spreadsheets). AI. Preliminary standard deviation estimates for BR and AS are 1.Screening Design Assignment
Choose a PlackettBurman screening design to identify the most important factors affecting BR and AS. AC.1 %. du Pont de Nemours and Company
. the next design might be preferable. respectively. Generate the response data using the simulator: %GLYXEL Examine the results in detail.
circle if significant
Team
1 2 3 4 5 6 7 8 9 10
DuPont Quality Management and Technology © 2000 E.Workshop 2: Glyxel Screening . Error (Resid.Team Reports
Effects for BEND RESISTANCE . I.11.6 Revised 5/09/2000
TP
AC
AI
CA
RP
DT
ET
QT
QF
PT
ST
BL
Exp. SD)
. du Pont de Nemours and Company SOE/MTB .
circle if significant
Team
11 12 13 14 15 16 17 18 19 20
DuPont Quality Management and Technology © 2000 E. SD)
.11. I. Error (Resid.7 Revised 5/09/2000
TP
AC
AI
CA
RP
DT
ET
QT
QF
PT
ST
BL
Exp.Team Reports
Effects for BEND RESISTANCE .Workshop 2: Glyxel Screening . du Pont de Nemours and Company SOE/MTB .
du Pont de Nemours and Company SOE/MTB .11.Workshop 2: Glyxel Screening .8 Revised 5/09/2000
TP
AC
AI
CA
RP
DT
ET
QT
QF
PT
ST
BL
Exp.circle if significant
Team
1 2 3 4 5 6 7 8 9 10
DuPont Quality Management and Technology © 2000 E. Error (Resid.Team Reports
Effects for AREA SHRINKAGE . SD)
. I.
9 Revised 5/09/2000
TP
AC
AI
CA
RP
DT
ET
QT
QF
PT
ST
BL
Exp. du Pont de Nemours and Company SOE/MTB .Workshop 2: Glyxel Screening . I.Team Reports
Effects for AREA SHRINKAGE . Error (Resid.circle if significant
Team
11 12 13 14 15 16 17 18 19 20
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.11.
10 Revised 5/09/2000
.Team Reports
Circle Factors To Be Studied in Workshop 3
Team
1 2 3 4 5 6 7 8 9 10
(note that a maximum of 5 factors may be circled)
TP TP TP TP TP TP TP TP TP TP AC AC AC AC AC AC AC AC AC AC AI AI AI AI AI AI AI AI AI AI CA CA CA CA CA CA CA CA CA CA RP RP RP RP RP RP RP RP RP RP DT DT DT DT DT DT DT DT DT DT ET ET ET ET ET ET ET ET ET ET QT QT QT QT QT QT QT QT QT QT QF QF QF QF QF QF QF QF QF QF PT PT PT PT PT PT PT PT PT PT ST ST ST ST ST ST ST ST ST ST BL BL BL BL BL BL BL BL BL BL
COMMENTS
DuPont Quality Management and Technology © 2000 E.11.Workshop 2: Glyxel Screening . I. du Pont de Nemours and Company
SOE/MTB .
Team Reports
Circle Factors To Be Studied in Workshop 3
Team
11 12 13 14 15 16 17 18 19 20
(note that a maximum of 5 factors may be circled)
TP TP TP TP TP TP TP TP TP TP AC AC AC AC AC AC AC AC AC AC AI AI AI AI AI AI AI AI AI AI CA CA CA CA CA CA CA CA CA CA RP RP RP RP RP RP RP RP RP RP DT DT DT DT DT DT DT DT DT DT ET ET ET ET ET ET ET ET ET ET QT QT QT QT QT QT QT QT QT QT QF QF QF QF QF QF QF QF QF QF PT PT PT PT PT PT PT PT PT PT ST ST ST ST ST ST ST ST ST ST BL BL BL BL BL BL BL BL BL BL
COMMENTS
DuPont Quality Management and Technology © 2000 E.11. du Pont de Nemours and Company
SOE/MTB .11 Revised 5/09/2000
.Workshop 2: Glyxel Screening . I.
Section 12
RESPONSE SURFACE DESIGNS
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SOE/MTB  12.1 Revised 9/26/2000
EVOLUTION OF THE ENVIRONMENT: Advanced Stage
SCREENING DESIGNS INTERACTION DESIGNS
RESPONSE SURFACE DESIGNS
Evolution of the Experimental Environment
NUMBER OF FACTORS OBJECTIVE COMMON DESIGNS
6 or more 38 26
Identify key factors
Understand factor interactions Full Factorial Fractional Factorial (resolution 5)
Prediction model Optimization BoxBehnken Central Composite Face Center Cube
PlackettBurman Fractional Factorial (resolution 3 or 4)
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USES OF RESPONSE SURFACE MODELS
Quantitative Understanding Prediction Optimization Conditions for Stability Calibration Process Control Adjustments
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FACECENTERED CUBE DESIGN for 3 factors
X3
Block 1 (First HalfFraction) Block 2 (Second Half Fraction) Block 3 (Face Points) Center Points
X2 X1
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BOXBEHNKEN DESIGN for 3 factors
X3
Edge Centers Center Point
X2 X1
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SETTING UP A RESPONSE SURFACE EXPERIMENT Assess the Environment Consider the Factors Consider the Responses Choose an Appropriate Design Consider Strategies for Bias Error Rewrite the Experimental Schedule in Physical Units Review the Experiment for Operability Avoid Blunders Plan for the Analysis Report the Recommendations
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company SOE/MTB  12.22 Revised 9/26/2000
RESPONSE SURFACE DESIGNS: Summary
Quadratic Polynomial Models Danger of Extrapolation Shape of Experimental Region
– Cubical: FaceCentered Cube
Link to Model Diagnostics Link to RS Example
Link to RS Workshop – Spherical: Central Composite, BoxBehnken
SpaceFilling, Balanced, and Robust
SOE/MTB  12.28 Revised 9/26/2000
DuPont Quality Management and Technology © 2000 E. I. du Pont de Nemours and Company
13.2 Revised 7/02/2000
.UNDERLYING ASSUMPTIONS
Fitted model form is “approximately correct”
– More important for Response Surface models
Deviations from model have no systematic component (bias error) Experimental error (random error) is approximately normally distributed SD of experimental error is homogeneous throughout experimental space
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I. du Pont de Nemours and Company
SOE/MTB .13.DIAGNOSTICS AND REMEDIES
ASSUMPTION Correct model form DIAGNOSTIC TOOL Lackoffit test POSSIBLE REMEDY Model augmentation Transformation
No bias error
Residual plots
Bias modeling Outlier handling
Normal error
Residual histogram & normal plot Fundamental knowledge
Transformation
Homogeneous error
Residual plots Fundamental knowledge
Transformation Weighted regression
DuPont Quality Management and Technology © 2000 E.3 Revised 7/02/2000
.
12 Revised 7/02/2000
. Variables
DuPont Quality Management and Technology © 2000 E. Available plots of residuals include:
Histogram Normal Probability Plot vs. I. Standardized and “Deleted” residuals use a standard deviation scale. Fits (Predicted Values) vs. Time vs. du Pont de Nemours and Company SOE/MTB . or Studentized [“Deleted”].13.RESIDUAL PLOTS IN MINITAB Minitab can calculate 3 kinds of residuals: Regular. Standardized.
• Store results of transformations in separate columns so that original values are retained.13.Minitab: Transformations • Transformations in Minitab are calculated using the Calculator… item in the Calc pulldown menu.
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.
13. du Pont de Nemours and Company SOE/MTB .
DuPont Quality Management and Technology © 2000 E. I. Minitab will not display RSquared values for the analyses of 2level designs but will display them for response surface designs.14 Revised 7/02/2000
.RSquared & Adjusted RSquared Both estimate percent or proportion of observed variability explained by model Rsquared adjusted is generally a more honest appraisal as it adjusts for the number of terms in the model.
14. I. du Pont de Nemours and Company
SOE/MTB .Section 14
RESPONSE SURFACE EXAMPLE
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.
du Pont de Nemours and Company SOE/MTB . The compound is added to a fixed amount of formula and the coating process completed.
Du Pont Quality Management and Technology © 2000 E. Three factors are under consideration: Factor ADDITIVE AMOUNT REACTION TIME REACTION TEMPERATURE Range 0 to 70 grams 20 to 60 minutes 100 to 180 degrees C
The yield of the compound is measured. Adhesion is then measured. I.2 Revised 1/30/2001
. Resources are available for a maximum of 24 runs. Specifications on the responses are: YIELD ≥ 91% ADHESION ≥ 45 grams Find settings of the factors for which these conditions can be achieved.RESPONSE SURFACE EXAMPLE Problem Statement
A new compound is being developed for a coating process.14.
14. du Pont de Nemours and Company
SOE/MTB . I.Du Pont Quality Management and Technology © 2000 E.3 Revised 1/30/2001
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14.4 Revised 1/30/2001
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SOE/MTB .
Du Pont Quality Management and Technology © 2000 E.14. I.5 Revised 1/30/2001
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17 Revised 1/30/2001
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EXAMPLE DATA PLOTTED ON CUBES
YIELD
50 77 Temperature 40 92 68 80 81 75 68 Additive
Du Pont Quality Management and Technology © 2000 E.41.82. 87. 85.42
31 44
75
65
51
3 Additive
40
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. I.85
37 41 24 38 10
37. du Pont de Nemours and Company
ADHESION
90 40 44 39 Temperature 48 31
75
82.40.
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27 Revised 1/30/2001
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SOE/MTB .Du Pont Quality Management and Technology © 2000 E.
90 6.000 0.55 4.067
P 0.6964 0.9%
RSq(adj) = 97.70 25.026 Coef 84. Estimated Regression Coefficients for YIELD Term Constant Additive Time Temperat Additive*Additive Time*Time Temperat*Temperat Additive*Time Additive*Temperat Time*Temperat S = 2.7162 T 121.61 1463.21 487.61 1463..75 13.141 0.000 0.50 0.649 9. Temperature The analysis was done using coded units.64 8.9%
Analysis of Variance for YIELD Source Regression Linear Square Interaction Residual Error LackofFit Pure Error Total .71 656.. Time.000 0. I.2216 0.80 12.86 1.320 0.33 3787.29 Revised 1/30/2001
DF 9 3 3 3 10 5 5 19
Seq SS 3746.62 5.Response Surface Regression: YIELD versus Additive.700 53.104 3.36 0.6406 0.75
Adj SS 3746.240 0.847 1.403 7.6406 0.849 0.7162 0. du Pont de Nemours and Company SOE/MTB .
Du Pont Quality Management and Technology © 2000 E.000 0.694
.047 18.210 0.340 6.00 41.2216 1.84 4.04 15.000 0.991 1.2216 1.33
Adj MS F 416.734
RSq = 98.000 0.302 101.530 1.7162 0.29 542.249 10.667 118.45 218.538 132.40 0.6406 1.000 0.25 SE Coef 0.349 P 0.70 25.000 0.000 0.14.10 1627.000 0.00 41.71 656.10 1627.04 15.
60 2.970 5.04 115.030 0.59 0.27 847.0256 1.6013 0.526 1. Time.000 0.000 40.577 0.831 P 0.
Du Pont Quality Management and Technology © 2000 E.59 17.247 17.653 92.424 39.60 346.80 2.80 Adj SS 2399.5847 0.665
Unusual Observations for ADHESION Observation ADHESION Fit SE Fit Residual 3 37.576 2.8%
RSq(adj) = 97.467 P 0. Estimated Regression Coefficients for ADHESION Term Constant Additive Time Temperat Additive*Additive Time*Time Temperat*Temperat Additive*Time Additive*Temperat Time*Temperat S = 1.93 11.18 402.236 0.5378 0.90 5.87 1206.03R .33 2428.000 0.90 6.00 28.6013 0.25 0.50 SE Coef 0.000 0.000 0.241 0.59 17.200 139.09 0.000 0.236 R denotes an observation with a large standardized residual.0256 0.14.. du Pont de Nemours and Company
St Resid 2.319 0.90 282.392 10.Response Surface Regression: ADHESION versus Additive.000 0.60 346.701 Coef 40.939 0.333 97.000 0.000 0.000 0.585 3.33 Adj MS F 266.93 11.000 0. I.67 3.00 28. Temperature The analysis was done using coded units.59 2.5378 1.7%
Analysis of Variance for ADHESION Source Regression Linear Square Interaction Residual Error LackofFit Pure Error Total DF 9 3 3 3 10 5 5 19 Seq SS 2399..
SOE/MTB .362 5.27 847.30 Revised 1/30/2001
.0256 1.893 2.425
RSq = 98.046 0.816 16.5378 0.87 1206.75 10.24 8.6013 T 68.
THOUGHT QUESTIONS Part 1
Do any of the initial design points satisfy the specified performance criteria for YIELD and ADHESION ? Which model terms are statistically significant ? What confidence level did you use to judge significance ? How well does the model fit the data ? How did you assess this ? At a given set of experimental conditions (X settings).31 Revised 1/30/2001
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. I. what is the experimental error in YIELD and ADHESION ?
SOE/MTB .14.
32 Revised 1/30/2001
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.14. I.Click on OK and then OK again in the next frame to get to:
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Overlaid contours for desired values of Yield, Adhesion
180
Lower Bound Upper Bound White area: feasible region
YIELD ADHESION
91 100
170
160
45 100
Temperature
150
140
130
120
110
100 0 10 20 30 40 50 60 70
Additive Hold values: Time: 60.0
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Link to RS Workshop
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du Pont de Nemours and Company
SOE/MTB .1 Revised 7/02/2000
.Section 15
WORKSHOP 3: Glyxel Response Surface
DuPont Quality Management and Technology © 2000 E. I.15.
Workshop 3 . Here we will study in more detail the key factors identified through your screening design. now we will use a response surface design to optimize the process.3 % Reactor Pressure (RP) 100 150 psi Dryer Temperature (DT) 120 150 °C Extruder Temperature 180 190 °C Quench Water Temperature (QT) 10 15 °C Quench 10 20 l/min SOE/MTB .2 Press Temperature (PT) 140 160Revised 7/02/2000 °C
(ET) Water Flow Rate (QF)
DuPont Quality Management and Technology © 2000 E.2 % impurity Catalyst Amount (CA) 0.Problem Description
This workshop is a continuation of the Glyxel problem described in workshop 2.7 3. The original list of factors examined in workshop 2 are given below.1 0. however. Factors (original list) Throughput (TP) Impurity (AI) Low Limit High Limit Units 200 800 kg/hr Additive A Concentration (AC)4 8 % Additive A 0. From your previous assignment you reduced this list down to the critical few variables (up to 5) to investigate in this response surface design. I.15. du Pont de Nemours and Company
.
Area Shrinkage (AS) (1. lower is better) Low shrinkage is required to maintain dimensional stability through customers’ processing. Such variables may include uncontrolled. du Pont de Nemours and Company SOE/MTB . noise.
Additionally. recall that based on acceptable profitability and market demand expectations we need to satisfy property goals with the highest possible throughput. we may choose to explicitly control them within the context of a designed experiment to understand their potential impact on product properties.15. I. target of 68) Gives a proper balance between enduse strength and customer processing needs. ambient. raw materials. refer back to the original problem description (Section 11 .(acceptable range 65 .3 Revised 7/02/2000
. Which factors explored in the Glyxel problem in workshop 2 are environmental variables? It is also possible that some factors retained for the optimization study in this workshop are environmental variables.workshop 2 background information slides) to refresh your memory on the design variable descriptions. What are they? The importance of Identifying environmental factor(s) and understanding their nature and how they might be treated during optimization will become clear in the assignment discussion and thought questions. Bend Resistance (BR) .Background Information
If needed.71 psi. Recall the two critical property goals.Workshop 3 . Although environmental variables are not typically controlled in operation.
DuPont Quality Management and Technology © 2000 E. or customer use variables. It was previously stated that we needed to achieve at least 500 kg/hr if possible with higher levels being more desirable.0% maximum. Several of the factors originally described fall into the category of environmental variables.
This simulator will ask for settings for your fixed factors. Recall that you want to detect a 3 psi change in BR and a 0. Which estimate would you use in your design size or sensitivity calculations here and why? Type BR and AS as column names for two unused columns in the worksheet. Verify that your intended design will be large enough to detect the size effects we are interested in. the preliminary estimates (given in workshop 2) and the estimates obtained from the screening design.
DuPont Quality Management and Technology © 2000 E. I. Examine the results in detail to understand which effects are important and how well the model fits. and the number of replicates. Generate the response data with the simulator by typing: %GLYXELRS in the session window.15.Workshop 3 .2% change in AS. Proceed to analyze. Fill in your teams results on the appropriate row in the BR and AS regression model results spreadsheets and answer all thought questions (slide 7) prior to generating any contour plots. You now have 2 standard deviation estimates for BR and AS. Choose either a CENTRAL COMPOSITE or BOXBEHNKEN design. Design sizes will vary according to the number of factors studied. design type. du Pont de Nemours and Company
SOE/MTB .4 Revised 7/02/2000
.RS Design Assignment (Part 1)
Select a response surface design. Enter * for factors that are in the design.
I.15.5 Revised 7/02/2000
. Finally. Wait for instructions on how to collect and process the confirmatory runs. and results obtained from confirmatory runs.Workshop 3 . you may want to investigate the range of environmental factor(s) either as onaxis or offaxis variable(s). Obtaining independent data for validation is a critical step for building confidence in the predictive capabilities of our models in the region of interest. Also.RS Design Assignment (Part 2)
Generate a few contour plots to get a feel for the behavior of the response surfaces. you may choose to relax this assumption and explore optimizing with regard to all factors (including environmental ones) . answer all thought questions on slide 12 and fill in your results on the team report spreadsheets with recommended settings. Keep in mind that knowing the key model effects can help point you to a more promising portion of the design space. Identify recommended factor settings (where predictions satisfy stated goals) to test model predictions with confirmatory runs. Next. du Pont de Nemours and Company
SOE/MTB . and recommendations. Try to identify design regions where property goals can be satisfied. be prepared to discuss (or assign a spokesperson from your team to discuss) your teams approach. predicted response levels.
DuPont Quality Management and Technology © 2000 E. Initially you may want to assume that any environmental factor(s) will vary across the full design range. to see if this makes a difference in meeting process goals albeit recognizing greater control of such factors(s) may be required. Finally. Under this assumption you might begin by generating contour plots that leave environmental factor(s) as offaxis variables set to their midpoints and then explore the limits of other design factors to see if our property goals can be met. results.
Flowchart for Experimental Design and Analysis
Perform initial design size or sensitivity calculations Design the experiment Run the experiment on the process and enter the data Analyze the experimental data
– fit the model to the responses – determine the important effects and check model adequacy (examine the various tabular summaries and residuals.15. any evidence of LOF?) – model look OK?
Generate plots describing the model
– 2D and 3D contour plots – do any predictions from the 2D contour plots satisfy process goals? – optimize the individual responses and then simultaneously optimize to meet the combined process goals
Verify predictions with check point runs
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what is the experimental error in BR and AS (in terms of a standard deviation)? Based on your results. which factors or set of factors would you choose as onaxis factors in contour plots?
SOE/MTB . I. Is there evidence of lack of fit? At a given set of experimental conditions (X settings).15.Thought Questions for Workshop 3
(Before contour plotting)
Do any of your initial design points satisfy the property and process goals? Which model terms are statistically significant? What confidence level did you use to judge significance? How well does the model fit the data? Be prepared to justify your answer. du Pont de Nemours and Company
.7 Revised 7/02/2000
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15.Response Surface Model Results (BR)
Design Used Significant Effects (list factor abbreviations) Main Effects Inter. du Pont de Nemours and Company
SOE/MTB .8 Revised 7/02/2000
. I. Effects Resd SD Rep SD
2 RAdj LOF?
Team
1 2 3 4 5 6 7 8 9 10
Resids OK?
DuPont Quality Management and Technology © 2000 E. Effects Quad.Workshop 3 .
du Pont de Nemours and Company
SOE/MTB . Effects Quad. I.Response Surface Model Results (BR)
Design Used Significant Effects (list factor abbreviations) Main Effects Inter. Effects Resd SD Rep SD
2 RAdj LOF?
Team
11 12 13 14 15 16 17 18 19 20
Resids OK?
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.Workshop 3 .15.
15. Effects Quad. du Pont de Nemours and Company
SOE/MTB . I. Effects Resd SD Rep SD
2 RAdj LOF?
Team
1 2 3 4 5 6 7 8 9 10
Resids OK?
DuPont Quality Management and Technology © 2000 E.Response Surface Model Results (AS)
Design Used Significant Effects (list factor abbreviations) Main Effects Inter.10 Revised 7/02/2000
.Workshop 3 .
du Pont de Nemours and Company
SOE/MTB .15.11 Revised 7/02/2000
. Effects Resd SD Rep SD
2 RAdj LOF?
Team
11 12 13 14 15 16 17 18 19 20
Resids OK?
DuPont Quality Management and Technology © 2000 E. Effects Quad.Response Surface Model Results (AS)
Design Used Significant Effects (list factor abbreviations) Main Effects Inter.Workshop 3 . I.
if any. on the impact the environmental factor(s) may have on meeting your process goals? What recommendations would you make. to improve the process by exercising greater control of the environmental factor(s)? What plot(s) and / or tables would you include in a report of your results?
SOE/MTB . if any.15.Thought Questions for Workshop 3
(After contour plotting)
Which contour plot(s) were the most informative? What is the most promising region of the design space for satisfying the property goals? Are throughput levels OK? What confirmatory (check point) runs did you make? Were your predictions supported? Requirements met? What conclusions can you make.12 Revised 7/02/2000
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15.Workshop 3 (Glyxel Response Surface) .13 Revised 7/02/2000
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SOE/MTB .Team Reports
Recommended Settings (use MP for MidPoint of excluded factors) Team
1 2 3 4 5 6 7 8 9 10
Predicted BR AS
Obtained BR AS
TP
AC
AI
CA
RP
DT
ET
QT
QF
PT
ST
DuPont Quality Management and Technology © 2000 E. I.
Team Reports
Recommended Settings (use MP for MidPoint of excluded factors) Team
11 12 13 14 15 16 17 18 19 20
Predicted BR AS
Obtained BR AS
TP
AC
AI
CA
RP
DT
ET
QT
QF
PT
ST
DuPont Quality Management and Technology © 2000 E.15.Workshop 3 (Glyxel Response Surface) .14 Revised 7/02/2000
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I.Section 16
OTHER EXPERIMENTAL ENVIRONMENTS
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SOE/MTB .16.
16.SOME OTHER TYPES OF EXPERIMENTAL SITUATIONS Categorical factors with more than 2 levels Constrained regions Mixture problems Incomplete block designs Split plot designs Nested designs Supersaturated designs
FOR THESE TYPES OF SITUATIONS CONSULT AN EXPERT!
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.
16.3 Revised 7/02/2000
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.CATEGORICAL FACTORS WITH MULTIPLE LEVELS
Catalysts Electronic components Suppliers Operators Machines Brands or types of formulation ingredients
SOE/MTB .
16. I.MIXTURE EXAMPLES
Drugs Gasoline Blends Metal Alloys Rocket Propellants Aerosol Propellants Herbicides
Paints Dyes Textile Fiber Blends Concrete Cake Mixes Composite Materials
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SOE/MTB .16. I.5 Revised 7/02/2000
.A CLASSIC MIXTURE
5 Parts Gin 1 Part Vermouth
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16.6 Revised 7/02/2000
.MIXTURE CONSTRAINT
0 ≤ Xj ≤ 1
Σ X =1
j j=1
q
so Xq = 1
ΣX
j=1
q1
j
Mixture Components Cannot Be Varied Independently Factorial and Response Surface Designs Cannot Be Used
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SOE/MTB . I.
I.FACTOR SPACE IN TWO VARIABLES
+
Independent
Mixture
1
X2
X2

0
X1
+
0
X1
1
FACTOR SPACE IN THREE VARIABLES
Independent X3 Mixture X3 X1+X2+X3=1 X2 X1
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.16.7 Revised 7/02/2000
X2 X1
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16.1.0.0.1.0.0
1. I.0.0
0.FACTOR SPACE FOR A FOURCOMPONENT MIXTURE
0. du Pont de Nemours and Company
SOE/MTB .8 Revised 7/02/2000
.1
DuPont Quality Management and Technology © 2000 E.0.0.0
0.
X1) = X2 .X2) = X1 . I.X1*X2 X22 = X2*X2 = X2(1 .QUADRATIC RESPONSESURFACE MODEL FOR TWO FACTORS Y = a0 + a1X1 + a2X2 + a12X1X2 + a11X12 + a22X22 The Mixture Constraint X1 + X2 = 1 X12 = X1*X1 = X1(1 .X1*X2 Quadratic Mixture Model (Scheffé) Y = b1X1 + b2X2 + b12X1X2
DuPont Quality Management and Technology © 2000 E.16.9 Revised 7/02/2000
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25*b12 b2
b1
X1 X2
1.10 Revised 7/02/2000
.0
0.5 0.16. I. du Pont de Nemours and Company
SOE/MTB .5
0.0
DuPont Quality Management and Technology © 2000 E.0 0.0 1.TWOCOMPONENT MIXTURE Scheffé Linear & Quadratic Model
Y
d = 0.
du Pont de Nemours and Company
SOE/MTB .THREECOMPONENT MIXTURE DESIGN
X1 = 1 Pure Component Binary Blend Ternary Blend Check Points
X2 = 1
X1 = 0
X3 = 1
DuPont Quality Management and Technology © 2000 E. I.16.11 Revised 7/02/2000
.
16.6 0.6
*
* 0.4 0. 0.3.0
0.5
0.7 0.6 0. du Pont de Nemours and Company SOE/MTB . I.9 0.0
*
* 0.3 0.0 0.12 Revised 7/02/2000
.1
X2
1.7 0.2 0.1 0.5)
* 1000 *
0.0
X3
DuPont Quality Management and Technology © 2000 E.5 0.ROCKET PROPELLANT CONTOUR PLOT
0.3 0.4 0.9
*1.2.0
0.4 0.2
800
0.0
* 700 800 900 * 1000
0.8 0. 0.5 0.3
Maximum Near (0.9 1.8 0.8 0.2 0.7
*
0.1 0.
13 Revised 7/02/2000
.MINIMUM COMPONENT LEVELS
Concrete Cake Steel
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SOE/MTB .16. I.
du Pont de Nemours and Company
.MINIMUM COMPONENT LEVELS
X2 = 0.5 0.14
0.0
X1 = 1
Requirements :
X1 ≥ 0.18 X2 ≥ 0.11
0.14 Revised 7/02/2000
X3 = 0.18
X2 = 1
0.5
0.0
X3 = 1
SOE/MTB . I.16.0 0.11
DuPont Quality Management and Technology © 2000 E.14 X3 ≥ 0.5
X1 = 0.
0 0.0
X1 = 1
X2 = 0.51 0.18 ≤ X1 ≤ 0.18
X2 = 1
0.16.15 Revised 7/02/2000
.5 0. du Pont de Nemours and Company
X3 = 0.58
SOE/MTB .0
X3 = 1
X3 = 0.52
0.11 ≤ X3 ≤ 0.14 ≤ X2 ≤ 0.58
Requirements :
X2 = 0.MINIMUM AND MAXIMUM COMPONENT LEVELS
0.14
0.5
0.51
X1 = 0.11
DuPont Quality Management and Technology © 2000 E.52 0.5
X1 = 0. I.
16 Revised 7/02/2000
.FLARE EXPERIMENT: DESIGN
X2 = NaNO3
Vertices Face Centers Center
X3 = SrNO3
X1 = Mg
X4 = Binder
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SOE/MTB .16. I.
16.17 Revised 7/02/2000
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SOE/MTB .AEROSOL PROPELLANT STUDY
X1 = 1
Mixture Highly Flammable
X2= 1
X3 = 1
DuPont Quality Management and Technology © 2000 E.
18 Revised 7/02/2000
. I.EXAMPLE OF CONSTRAINED REGION: Petroleum Fractionation Process
Amount of Toluene In Solvent
Equipment Fouling: No Phase Separation
Region of Interest Unfavorable Economics Solvent/Solute
DuPont Quality Management and Technology © 2000 E.16. du Pont de Nemours and Company
SOE/MTB .
19 Revised 7/02/2000
.STEPS FOR DESIGNS IN IRREGULAR REGIONS
Define Region Incorporate the Principles of Good Design Identify Candidate Runs
– Include extreme points
Select Runs
– By inspection. du Pont de Nemours and Company
SOE/MTB . I.16.g. DOptimal Design)
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20 Revised 7/02/2000
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SOE/MTB .16.OTHER EXPERIMENTAL ENVIRONMENTS: Summary
Discrete Factors Mixture Designs Constrained Factor Spaces
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Section 18
SUMMARY
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SOE/MTB .18.
I.18.2 Revised 3/10/2000
. du Pont de Nemours and Company
SOE/MTB .EXPERIMENTAL DESIGN VERSUS ONEFACTORATATIME EXPERIMENTS
Drawbacks of onefactoratatime experiments
– Not spacefilling – Ignores interactions – Ignores experimental error – Inefficient due to lack of hidden replication – Limited system understanding – Potential bias error due to lack of randomization
DuPont Quality Management and Technology © 2000 E.
18. du Pont de Nemours and Company SOE/MTB .EXPERIMENTAL DESIGN VERSUS ANALYSIS OF HISTORICAL DATA
Drawbacks of historical data analysis
– Correlations between factors – Unrecorded control actions may create misleading effects.3 Revised 3/10/2000
. I. confusion of cause and effect – Typical lack of boldness in factor settings – Data collection problems
– Missing data – Bad observations
– Large bias errors due to lack of randomization – At best describes “What is” instead of “What is possible”
DuPont Quality Management and Technology © 2000 E.
4 Revised 3/10/2000
. I.WHEN SHOULD I USE DOE ? Discovery Research and Scouting Product/Process Design and Development Process Scaleup. Startup. and Qualification Process Control and Calibration Product/Process Improvement
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SOE/MTB .18.
number & nature of factors) Balanced Statistical Designs Measure All Relevant Responses BiteSized Experiments Boldness Randomization and Blocking Estimate Experimental Error Avoid Blunders Plan Ahead for Statistical Analysis
DuPont Quality Management and Technology © 2000 E.PRINCIPLES OF GOOD EXPERIMENTAL STRATEGY Diagnosis of the Environment (objectives.5 Revised 3/10/2000
.18. prior knowledge. du Pont de Nemours and Company SOE/MTB . I.
Quadratic model: Y = b0 + b1X1 + b2X2 + b3X3 + b12X1*X2 + b13X1*X3 + b23X2*X3 + b11X12 + b22X22 + b33X32 Facecentered cube. . I. PlackettBurman and Fractional Factorial Usually only a few more runs than factors
Interaction Designs
Fewer factors Identify/exploit interactions Model contains linear terms and at least some interactions: Y = b0 + b1X1 + b2X2 + b3X3 + b12X1*X2 + b13X1*X3 + b23X2*X3 Full and Fractional Factorial
Response Surface Designs
Small number of factors (36) Used for prediction. . optimization.EXPERIMENTAL EVOLUTION
Screening Designs
Many factors Distinguish “critical few” from “trivial many” Linear model: Y = b0 + b1X1 + b2X2 + b3X3 + b4X4 + . others
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SOE/MTB . modelling. .6 Revised 3/10/2000
.
du Pont de Nemours and Company
. Document & Communicate Business Results
SOE/MTB .DOE APPLICATION PROCESS
Strategy of Experimentation
Identify Business Needs Gather Information Define Experimental Objectives Design the Experiment Run Experiment Analyze Experiment Interpret Results Perform Confirmation Runs Go to Next Stage of Experimentation? Apply Results Assess. I.18.7 Revised 3/10/2000
Update Information
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ANALYZING EXPERIMENTS: Flowchart
Screening Designs Inter action Designs
ENTER DATA DISPLAY DATA PLOT/VERIFY DATA FIT MODEL
Response Sur face Designs
Main Effects
Main Effects and Interactions
ASSESS SIGNIFICANCE VALIDATE ANALYSIS PLOT RESULTS
Quadratic Model
Rank Effects
Exploit Interactions
Find “ Optimum”
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SOE/MTB .
assuming no change in process other than possibly a level shift (use blocking) between when the existing and new data are collected
Do not overuse doptimal designs. I.
DuPont Quality Management and Technology © 2000 E.18.9 Revised 3/10/2000
. Use standard designs whenever they are appropriate. du Pont de Nemours and Company SOE/MTB .WHEN DO I NEED A DOPTIMAL DESIGN ?
You may need a doptimal design for the following situations:
– Discrete/Qualitative factors at more than 2 levels – Constrained regions (including mixtures) – A special model (mixed number of levels of factors or models with some terms excluded due to your assuming that they have negligible effects on the responses of interest) – To augment an existing design to be able to estimate a larger model (in some cases) .
Section 19
MIXTURES IN MINITAB
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all ( 1 3 . ½) blends. 2 3 ) blends
Extreme vertices
– use when components have upper bounds
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SOE/MTB 19. I. 1 3 . …
Simplex lattice
– use when components have no upper bounds (lower bounds are OK) – includes:
• degree 1 design: pure component runs • degree 2 design: pure component runs.2
Revised 07/02/2000
.TYPES OF MIXTURE DESIGNS AVAILABLE IN MINITAB
Simplex centroid
– use when components have no upper bounds (lower bounds are OK) – includes:
• 2q1 runs for q components • all pure component (100% of component) runs. ternary runs.
I.3
Revised 07/02/2000
. select DOE Mixture Create Mixture Design Select the number of components Select the type of mixture design Click on Designs… to select the points to be included
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SOE/MTB 19.CREATING MIXTURE DESIGNS IN MINITAB
Start
a new Minitab project From the Stat pulldown menu.
11 to .18 to .4
Revised 07/02/2000
.14 to . du Pont de Nemours and Company
SOE/MTB 19. I.51 .EXAMPLE WITH LOWER AND UPPER BOUNDS ON COMPONENTS: Choose type of design
Effects X1 X2 X3 Ranges .58
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I.5
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SOE/MTB 19.Extreme Vertices Design Options: Vertices and Center Point only
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I.6
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. Center Point. Axial Points
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.Extreme Vertices Design Options: Vertices. I. Binary Blends
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I.51 . du Pont de Nemours and Company
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© 2000 E.EXAMPLE WITH LOWER AND UPPER BOUNDS ON COMPONENTS: Defining factors in Minitab
Effects X1 X2 X3
Ranges .8
Revised 07/02/2000
.
EXAMPLE WITH LOWER AND UPPER BOUNDS ON COMPONENTS:
Minitab worksheet from extreme vertices design with degree=2 and center point
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.
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SOE/MTB 19.VISUALIZING THE MIXTURE DESIGN IN MINITAB
After producing the design:
Select
from the Stat pulldown menu
DOE Mixture Simplex Design Plot
Click
OK to use
the default graph settings
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ANALYSIS OF MIXTURE DATA IN MINITAB
Select
from the Stat pulldown menu
DOE Mixture Analyze Mixture Design
Select The
the response column to analyze
default model is quadratic . du Pont de Nemours and Company
SOE/MTB 19.click OK
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. I.
8886 79.02%
Analysis of Variance for Response Source Regression Linear Quadratic Residual Error Total DF 5 2 3 7 12 Seq SS 1632.010 0.60 31.14 4.041 0.70 5.74 209.66 13.9732 23.86 49.75 P 0.73
(component proportions) Adj SS 1632.35 P * * * 0.000 0.0298 RSq = 98.012 0. X2.30 SE Coef 24.12
Revised 07/02/2000
.35 280.6776 4.33 160.86 71.697 SE Fit 1.35 T * * * 2.EXAMPLE WITH LOWER AND UPPER BOUNDS ON COMPONENTS: Minitab analysis results
Regression for Mixtures: Response versus X1.50 3.03 28.40R
R denotes an observation with a large standardized residual DuPont Quality Management & Technology
© 2000 E.44 77.26% Coef 44.42 20.67
PRESS = 85. du Pont de Nemours and Company
SOE/MTB 19.8406 Adj MS 326.83 62.5777 39.85%
RSq(adj) = 97.54 82.656 RSq(pred) = 94. X3 Estimated Regression Coefficients for Response (component proportions) Term X1 X2 X3 X1*X2 X1*X3 X2*X3 S = 2.26 9.027
Unusual Observations for Response Observation 1 Response 46. I.89 1561.012 VIF 243.697 St Resid 2.19 77.0328 28.84 1661.321 Residual 3.88 165.000 Fit 49.89 168.9464 71.1201 F 79.34 3.81 194.
select DOE Mixture Response Trace Plot
Click OK for default settings
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SOE/MTB 19.
From the Stat pulldown menu.13
Revised 07/02/2000
.EXAMPLE WITH LOWER AND UPPER BOUNDS ON COMPONENTS: Minitab Response Trace Plot
Minitab’s response trace plot is similar to an effects plot for mixture components.
I.14
Revised 07/02/2000
.EXAMPLE WITH LOWER AND UPPER BOUNDS ON COMPONENTS: Minitab contour plot
Produce a contour plot of the model fit by selecting from the Stat pulldown menu: DOE Mixture Contour/Surface (Wireframe) plots Click on Contour plot Setup OK (for default settings) 3D plots and optimizations are available also
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SOE/MTB 19. du Pont de Nemours and Company
Note that this plot was produced by requesting specific contour levels.
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SOE/MTB 19. I.THOUGHT QUESTION
What if sample sizes test tells you only need 8 design points .and each experiment will be very expensive.15
Revised 07/02/2000
. What would you do?
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– Variable 3 must be GREATER than 0. – Variable 2 must be less than 0.
You will need an extreme vertices design due to the maximums given for variables 1 and 2.MIXTURE EXAMPLE 2
Create a Mixture Design with the Following Constraints – Variable 1 must be less than 0.60.70.20.
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Revised 07/02/2000
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SOE/MTB 19. I.
MIXTURE EXAMPLE 2: 2 Design Alternatives
Minitab’s default design with axial points
Minitab’s degree=2 design without axial points
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© 2000 E.15 0. Poly 0.MIXTURE EXAMPLE WITH LINEAR CONSTRAINTS
Four factors with their ranges.15 0.10 to 0.05.55 to 0.00 to 0.30 Comp1 Comp2 Filler 0. I.85
We have the following additional constraints B + C <= 0.18
Revised 07/02/2000
. du Pont de Nemours and Company
SOE/MTB 19.15 B + C >= 0.00 to 0.
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SOE/MTB 19.MIXTURE EXAMPLE WITH LINEAR CONSTRAINTS: Define Variables
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Revised 07/02/2000
.
I.20
Revised 07/02/2000
.MIXTURE EXAMPLE WITH LINEAR CONSTRAINTS: Define Constraints
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SOE/MTB 19.
100 0.025 0.000 0.000 0.25 0.30 0.725 0.100 0. du Pont de Nemours and Company
.050 0.20 0.750 0.15 0.000 0.15 0.050 0.150 0.000 0.10 0.15 0.10 0.550
SOE/MTB 19.025 0.025 0.675 0.775 0.050 0.15 0.025 0.725 0.150 0.750 0.30 0.000 0.25 0.MIXTURE EXAMPLE WITH LINEAR CONSTRAINTS: Extreme Vertices with Axial Points
Run 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 Poly 0.000 Filler 0.10 0.050 0.150 0. I.675 0.10 0.625 0.100 0.025 0.025 0.25 0.050 0.30 Comp1 0.850 0.150 Comp2 0.050 0.21
Revised 07/02/2000
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© 2000 E.050 0.000 0.775 0.000 0.100 0.850 0.025 0.650 0.30 0.650 0.050 0.025 0.700 0.050 0.550 0.25 0.050 0.625 0.
20.1 Revised 5/08/97
. du Pont de Nemours and Company
SOE/MTB .Section 20
GLOSSARY OF TERMS
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the statistical significance of particular model terms or groups of terms can be tested using Fratios. such as Doptimality. balance Desirable characteristic of an experimental design wherein design points are allocated in a manner that is balanced with respect to the center of the factor space. centering The procedure of reexpressing the scale of a continuous factor by subtracting a central value.
DuPont Quality Management and Technology © 2000 E. BoxBehnken designs A particular class of response surface designs which are spherical in shape. central composite in cube design The same as a facecentered cube. central composite in sphere design A special class of central composite designs in which the axial points are located outside the faces of the cube. such as the midpoint of the factor’s experimental range. Syn: star points. Syn: systematic error. often due to a single assignable cause. 95%) associated with the interval represents the longrun percentage of times that the interval will actually include the population parameter. and are usually treated as unordered. blocking Running the experiment in specially chosen subgroups. on the surface of the circumscribed sphere. The confidence level (e. axial points. These are a special class of central composite designs in which the axial points are located in the centers of the faces of the cube. often using an algorithm tied to some particular optimality criterion.g. within which the experimental conditions or material is expected to be more homogeneous than between blocks. and the overall centroid. The levels may be numerical or nonnumerical labels. boldness The recommended practice in experimentation of investigating factors over wide ranges. confidence interval An interval within which an unknown population parameter is estimated to lie.GLOSSARY OF TERMS
algorithmic designs Designs that are computergenerated for very specific situations. Fitting polynomial models in the centered factors results in more easilyinterpreted coefficients. from the factor values. I. categorical factor A factor that can assume only a finite number of possible values or levels. bias error Variability in the response data that is of a systematic. du Pont de Nemours and Company
SOE/MTB . analysis of variance (ANOVA) Procedure for analyzing data which involves partitioning the total variation into portions explainable by a model and unexplainable. Through appropriate partitioning. patterned nature. and reduces correlations among the coefficients. central composite design A class of response surface designs which consist of corner points.20.2 Revised 5/08/97
. called blocks. Syn: discrete factor. axial points Points in a central composite design having the property that all but one of the factors are set at their middle level.
I. correlation A measure of the degree to which values of one variable change in concert with values of another variable. du Pont de Nemours and Company SOE/MTB .20. and points of constant response are connected by curves. contour plot A twodimensional plot of the relationship between two continuous factors and a response. discrete factor see categorical factor duplicate A repeated run that does not repeat all elements of the 'run' process.f. execution. Syn: noise factor. Syn: aliasing.g. design of experiments (DOE) A strategic process. for guiding the planning. 100% efficiency may not always be achievable. or setting conditions once and making multiple pieces of product and measuring each.f. The expected change in the response as you go from the low to high level of the factor/interaction/etc.3 Revised 5/08/97
.) or estimate experimental error (residual or replicate d. extrapolation Making predictions outside the range covered by the current data. When two effects are totally confounded they are inseparable from each other they are both estimated with the same contrast. Usually expressed as a percentage between 0 and 100. called contour lines. analysis. environmental factor Factor that may affect product functionality but is not controlled during normal production or use. Usually specified in a design table with factors assigned to columns and runs to rows which indicate the factor combinations to be run.) design The set of specific factor combinations to be run in the experiment. a theoretical optimum. efficiency A comparison of the current design vs. Examples: making one piece of product and measuring it more than once.
DuPont Quality Management and Technology © 2000 E.low level average. May be based on any of several commonlyused criteria (e. degrees of freedom (d. effect A difference of averages: high level average . continuous factor A factor which can take on any value over some numerical range. Defficiency or Gefficiency).) The number of independent pieces of information used to fit a model (model d. Usually generated algorithmically. or to compare variances. Doptimal design A design that minimizes the volume of the region of uncertainty of the unknown model parameters.GLOSSARY OF TERMS
confounding A property of a design wherein the estimates of certain effects are correlated with each other. Note distinction from replicate. with supporting methods and tools. and application of results of experimental or developmental programs. experimental error Lack of repeatability (variability) in the experimental outcomes. in which the plot axes represent the two factors. Ftest A ratio of variances or mean squares used to compare means.f. or to test the significance of terms or groups of terms in models.
Syn: independent variable. the reflection is obtained by reversing all ‘+’ and ‘’ signs in the coded design table. I. historical data Data taken during the normal operation of a process where factors are not varied in a deliberate. most commonly used in cases where the factors each have two levels. or the response value at that point. du Pont de Nemours and Company SOE/MTB . controlled variable. which may depend on either the location of the point in the design space.
DuPont Quality Management and Technology © 2000 E. lackoffit test An analysis that compares residual variability versus replicate variability to assess whether the model could somehow be significantly improved using the current data. planned manner.GLOSSARY OF TERMS
face centered cube design See central composite in cube design. linear model A model which includes main effects only. Various commonlyused measures are available. Gaussian distribution See normal distribution. highorder interactions Interaction terms that involve several (typically 3 or more) variables simultaneously. A foldover PlackettBurman design will isolate the main effects from twoway interactions.4 Revised 5/08/97
. inoperable region A subset of the design space in which response data can not be collected/used.20. predictor. Frequently used as a basis for blocking or determining fractional factorial designs. hidden replication The apparent repeating of factor combinations when a balanced design is collapsed over variables not involved in the effect of interest. interaction A condition involving two or more factors in which the effect of one factor depends on the levels of the other(s). factor A variable which is deliberately manipulated in an experiment. input variable. knob. interaction model A model which consists of main effects and 2factor interactions (higherorder interactions generally not included). foldover design A design obtained by adding the reflection of a design to the original design (thereby doubling the number of runs). interpolation Making predictions within the range covered by the current data. or both. influence A numerical measure of the importance of an observation in determining the fitted model. mean The average. fractional factorial design Subset of a fullfactorial design that is formed by totally confounding factor effects with certain highorder interactions. Syn: reflected design. factorial design Experimental design that is generated by using all possible combinations of each of the levels of the factors.
which is varied across a range. parameter An unknown constant associated with the population. outlier An observation that appears to be far removed from the range of variation of the other observations in the data set.20. quadratic model A continuous factor model which consists of main effects. This process is then repeated in turn for each factor. pvalue of an estimated effect The probability of observing an effect that large purely by chance i. population The hypothetical set of all possible data values of a variable. and curvature terms in each factor. Syn: Gaussian distribution. practical significance The degree to which an estimated effect or parameter represents something meaningful or useful in the context of the experimental environment. normal distribution A symmetric. model A mathematical representation of the relationship between the factors and the response.e. often used to model the distribution of random error. onefactoratatime experimentation An experimental strategy which involves holding all factors constant except one. orthogonal design A design in which the columns of the design matrix are uncorrelated with each other. 2factor interactions. when the true effect is actually zero. regardless of their significance.5 Revised 5/08/97
. Factor effects are not completely independent of 2factor interactions. du Pont de Nemours and Company
SOE/MTB . Assumes that the true variance is about the same for all factor combinations in the experiment. orthogonal coding or scaling Expressing the range of a factor on a 1 to +1 scale.
DuPont Quality Management and Technology © 2000 E. Designs where the number of runs is a power of 2 should be treated as fractional factorials. bellshaped function that represents the expected frequency of data values. PlackettBurman design A class of twolevel screening designs that exist in multiples of 4 runs. quality The totality of features and characteristics of a product or service that bear on its ability to satisfy stated or implied needs. the stronger the evidence of a real effect. Also known as the coefficient of determination. Increases with the addition of model terms. It is specified by a mean and standard deviation.GLOSSARY OF TERMS
mixture experiment An experimental environment where the factors of interest are the proportions of various ingredients in a formulation. pure error standard deviation See replicate standard deviation. pooled standard deviation A combined estimate of experimental error variability based on replicating more than one set of experimental conditions. I. Rsquared The proportion of the total variation of the response explained by fitting the model. The smaller the pvalue. May suggest a possible error or anomaly.
Compares the variance explained by the model to the variance unexplained by the model. screening experiment A stage of experimentation where the experimenter needs relatively crude information about which of a relatively large number of factors are important.GLOSSARY OF TERMS
Rsquared adjusted An adjusted form of Rsquared that takes into account the number of terms in the model visavis the total number of observations.changing factor settings. regression Ftest A test that assesses the overall significance of the model. characteristic. Can be negative for models that have no value. Provides an estimate of the standard deviation of experimental error. provides an estimate of the standard deviation of experimental error. du Pont de Nemours and Company SOE/MTB . A design of resolution R is one in which no pfactor effect is confounded with any other effect containing fewer than Rp factors. robust Insensitive to changes in environmental conditions. making product. Quadratic models are typically used as the fitted models. calibration. response A variable which is observed/measured whose value may depend upon the settings of the design factors.) Note distinction from duplicate. etc. It can not be attributable to any single cause. I. Syn: dependent variable. residual The difference between an observed response value and the response predicted from the model. but will appear as random variation. Under the assumption that the fitted model form is valid. random error Variability in the response data which exhibits no systematic pattern.20. Models containing main effects only are typically used here.e. Provides a more equitable measure for comparing models of different sizes than the unadjusted Rsquared. reflected design See foldover design. resolution (of fractionalfactorial design) A number which indicates the level of confounding in a fractionalfactorial design. replicate standard deviation A pooled standard deviation computed using all replicated sets of runs.6 Revised 5/08/97
. Syn: pure error standard deviation. etc. residual standard deviation A standard deviation based on the set of all residual values. Higher numbers imply less confounding. measuring product. regression (least squares) A method of fitting a model to a set of data by minimizing the sum of squares of the deviations from the model. replicate A repeated run that includes repetition of all components of the 'run' process (i. response surface experiment A stage of experimentation where the experimental data is to be used for optimization. prediction. property. randomization The deliberate scrambling of the run order of the design so that any bias present is unlikely to be confounded with any factor effects.
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variable A measurement or observation for which any of various possible data values can occur.
DuPont Quality Management and Technology © 2000 E.7 Revised 5/08/97
. I. statistic A numerical characteristic of a sample. The square of the standard deviation. du Pont de Nemours and Company
SOE/MTB . standard deviation A measure of the variability in a population or set of data. studentized residual The residual divided by the estimated standard deviation of the residual where the current observation is omitted from the standard deviation calculation. variance A measure of the variability in a population or set of data. transformation A function applied to a variable (typically a response) to help improve the fit of the model.GLOSSARY OF TERMS
signaltonoise ratio Delta/s where delta is the minimum change in the response that is desired to be detected and s is the standard deviation of experimental error. statistical significance A conclusion made from statistical analysis of data that a difference or effect is real. The square root of the variance. mean and standard deviation. or to make the statistical analysis more valid. standard error The variability associated with an estimated effect or coefficient.20. for example. standardized residual The residual divided by the estimated standard deviation of the residuals where all observations contribute to the standard deviation.
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SOE/MTB 21.1
Revised: 5/08/2000
.Section 21
REFERENCE
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I.2
Revised: 5/08/2000
.CONTENTS
Catalogue of Designs Blank Cube Diagrams Defining Relations for FractionalFactorial Designs Miscellaneous Formulas Selected DOE Bibliography DOE Related Accession Reports Consultant List (handout)
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SOE/MTB 21.
DESIGN CATALOGUE: Twolevel Designs
Design
Full Factorial
Number of Distinct Points
2k
Confounding of Model Terms
none either total or none .see pages later in this section
Fractional Factorial 2km
PlackettBurman
multiples of 4 main effects partially that are not powers of 2 confounded w/interactions multiples of 8 main effects clear of 2factor that are not powers of 2 interactions
PlackettBurman plus Reflection
k = number of factors in design m = degree of fractionation
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Revised: 5/08/2000
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SOE/MTB 21.4
Revised: 5/08/2000
.DESIGN CATALOGUE: Response Surface Designs
Design
FaceCentered Cube BoxBehnken Spherical CentralComposites
Factor Levels
3 3 5
Shape of Design Space
Cubical Spherical Spherical
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I.23 FACTORIAL DESIGN
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SOE/MTB 21. I.TWO 23 FACTORIAL DESIGNS
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7
Revised: 5/08/2000
. I.33 FACTORIAL DESIGN
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SOE/MTB 21.
I.TWO 33 FACTORIAL DESIGNS
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SOE/MTB 21. I.THREEFACTOR FACECENTERED CUBE
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.
I.10
Revised: 5/08/2000
.TWO THREEFACTOR FACECENTERED CUBES
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Revised: 5/08/2000
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SOE/MTB 21. I.THREEFACTOR BOXBEHNKEN DESIGN
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. I.TWO THREEFACTOR BOXBEHNKEN DESIGNS
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Revised: 5/08/2000
.FRACTIONALFACTORIAL DESIGNS AVAILABLE WITH VARIOUS RESOLUTIONS
Number of Factors 3 4 5 6 7 8 9 10 11 12 Resolution III 4 8 8 8 16 16 16 16 Number of runs required for: Resolution Resolution IV V or more 8 16 16 16 32 32 32 32 16 32 64 64 128 128 128 256 Full Factorial 8 16 32 64 128 256 512 1024 2048 4096
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. I. .+(nk1)sk2 (n11)+(n21)+ .MISCELLANEOUS HANDY FORMULAS
Sample Mean Y=
Y1 + Y2 + . .+(nk1)
where n1 and n2 are the number of observations in the low and high “halves” of the factor effect.
Confidence Interval
estimate +/. the effect is statistically significant
Sample Pooled Variance sp2 =
where s12 . . . .t * standard error
t is a tabled Studentt quantile whose value depends on the degrees of freedom & confidence used When zero is not included in the confidence interval. . . .Ylow
about 50% more than for 2 levels
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For 3level designs
Estimated Effect
Yhigh . + (YnY)2 n1 (n11)s12+(n21)s22+ .14
Revised: 5/08/2000
. Yn n
=
ΣY
n i=1
Standard Error of a Factor Effect sFE = sp
i
n
√
1 +n n1 2
1
Sample Variance s2 =
(Y1Y)2 + (Y2Y)2 + . . . sk2 are the individual variances and n1 . . nk are the number of replicate measurements at each combination
Experiment Size
For 2level designs
Sample Standard Deviations
s=√ s2 sp = √ sp
2
n = 7 or 8
(
2
∆/s
)
where ∆ is effect size desired to detect and s = estimate of std dev. n2 . du Pont de Nemours and Company
SOE/MTB 21. . s22 . .
Y)2 i=1 R2 = _ n (Yi .MISCELLANEOUS HANDY FORMULAS (continued)
Explained Variation (%) in Regression (RSquared) _ n 100 (Ypredicted .(varianceresidual/ variancetotal))
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n
i
2 pred)
i=1 n
/(nk)
Σ
i=1
_ (Yi .Y)2 /(n1)
)
SOE/MTB 21. du Pont de Nemours and Company
. I.Y)2
Σ Σ
i=1
Explained Variation in Regression (RSquared adjusted) R2(adj) = 100
(
1
Σ(Y .15
Revised: 5/08/2000
where k = number of model terms (including constant) R2(adj)= 100 (1 .
William G. 1987. Inc. Box.
DuPont Quality Management & Technology
© 2000 E. 1990.SELECTED DOE BIBLIOGRAPHY
Design and Analysis of Experiments. Montgomery. John Wiley and Sons. Wilmington. George E. Virginia Polytechnic Institute and State University. Hess. Hunter and J. 1989. Inc. P. John Wiley and Sons. Experiments with Mixtures. Myers. Empirical Model Building and Response Surfaces. Inc. DuPont Quality Management & Technology Center.. 3rd ed. James L. du Pont de Nemours and Company
SOE/MTB 21. John Wiley & Sons. 1978. DE. Response Surface Methodology.. Raymond H. Box and Norman R. George E. Inc. Course Text (1988). Inc. Douglas C. John Wiley and Sons. Mason. Stuart Hunter. 1976. Robert L.16
Revised: 5/08/2000
. Richard F. Statistics for Experimenters. Statistical Design & Analysis of Experiments With Applications to Engineering and Science. 1990. I. John Cornell. Gunst. Draper. 2nd ed. P. Strategy of Experimentation. John Wiley and Sons.
– Accession Report #17960
Design of Experiments Quick Reference Guide
– Quick reference guide for trained users of DOE as a strategic process. I.17
Revised: 5/08/2000
.AVAILABLE DOERELATED MATERIALS
Design of Experiments: A Competitive Advantage
– Introduction in question and answer format – Accession Report #17934
Design of Experiments Application Guide
– Outline of DOE as a strategic process. Includes tools and methods. How and when to apply the tools and methods effectively. – Accession Report #17961
Design of Experiments Overview (presentation)
DuPont Quality Management & Technology
© 2000 E. du Pont de Nemours and Company
SOE/MTB 21. examples and catalogs.
du Pont de Nemours and Company SOE/MTB Revised 5/09/2000
.Glyxel Screening Response Surface Designs Model Diagnostics Response Surface Example Workshop 3 .Glyxel Response Surface Other Experimental Environments Algorithmic Design Summary Mixtures in Minitab Glossary of Terms Reference
Agenda Additions: Questions & Answers Your Data Session
DuPont Quality Management and Technology © 2000 E.TABLE OF CONTENTS
SECTION 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 TITLE Introduction Workshop 1 Foundations of the Strategy Factorial Geometry Factorial Example: Design Analysis of TwoLevel Factorial Designs Factorial Example: Analysis Good Experimental Practice Screening Designs Screening Example Workshop 2 . I.