Design Experiments Using Minitab

Yanling Zuo(), PhD Minitab Inc.

MINITAB DOE Overview

DOE menu

Factorial

MINITAB DOE Overview

Response Surface

Mixture

Minitab Inc., 2003

MINITAB DOE Overview

Taguchi

Minitab Inc., 2003

Case Study
A quality team is studying how a catalytic reaction converts substrate into a final product.

A sketch of the converter

Feed 100% Reactants

70% products, 30% reactants

Temperature

Rev/min catalyst

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Factors identified after brainstorming:

Feed rate Flow rate settings for feed tank (10,15 ml/min) Catalyst (A, B) Agitation rate (100, 120)

Temperature (140, 180 C)

Percent concentration (3%, 6%)

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Response: Percent of substrate reacted

Data collection:
The team has enough budget to perform 35 runs. They could run a full factorial design (25=32). However, a better approach is to run a fractional design, analyze results, and decide on subsequent experimentation. Whats next? Create a fraction design.

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Create the design with Minitab Go to Stat > DOE > Factorial >

Create Factorial Design

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Output

Note: Main effects confounded with 4-way interaction, 2-way interaction with 3-way interaction

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Worksheet

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Analyze the design with Minitab Go to Stat > DOE > Factorial > Analyze Factorial Design

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Normal Probability Plot of Effects

(response is Reacted, Alpha = .05)

99 95 90 80 70 60 50 40 30 20 10 5 1 DE E BD D B Effect Ty pe Not Significant Significant
F actor A B C D E N ame F eedrate C ataly st A gitation Temp C onc%

Normal Plot of the Effects

Percent

-10

-5

5 Effect

10

15

20

Lenth's PSE = 1.875

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Pareto chart of Effects
(response is Reacted, Alpha = .05) 4.82
B D BD DE E
F actor A B C D E N ame F eedrate C ataly st A gitation Temp C onc%

Pareto Chart of the Effects

Term

CE A BC AB AE BE AD AC CD C

0 Lenth's PSE = 1.875

10 Effect

15

20

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Significant factors: Catalyst (B)

Temp (D)
Concentration (E) Catalyst x Temp (BD) Temp x Concentration (DE) Whats next: Remove non-significant effects and refit models.

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Output:

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Estimated coefficients:

Reacted = -88.37 32.75 x Catalyst + 1.02 x Temp +23.25 x Conc + 0.27 x Catelyst x Temp -0.16 x Temp x Conc. (Can be used to predict percent reacted settings)

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Residual plots
Residual Plots for Reacted
Normal Probability Plot
99 90 4

Versus Fits

Residual
-5.0 -2.5 0.0 Residual 2.5 5.0

Percent

50 10 1

2 0 -2 -4 50 60 70 80 Fitted Value 90

Histogram
4 4

Versus Order

Frequency

Residual
-4 -2 0 Residual 2 4

3 2 1 0

2 0 -2 -4
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16

Observation Order

Whats next?
Create factorial plots to find best settings.

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Factorial Plots

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C atalyst

Interaction Plot for Reacted

Data Means
180 140 3 6 90

75

Catalyst A B

60 90

75

Temp 140 180

Cube Plot (data means) for Reacted

47.0 80.0

T emp 60

C onc%

64.5 180

94.0

Temp

55.5

66.0 6 Conc% 3

53.0 140 A Catalyst

62.0 B

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Conclusions: Feed rate and agitation do not have a significant impact

Catalyst B, a temperature of 180C, and 3% concentration maximize substrate consumption.

Followup experiment: The team had budget for 19 additional runs. They used Catalyst B and run a 22 full factorial design with 2 center points to detect curvature in the response. They centered experiment at currently known optimal settings,180C, 3%.

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Numerical output for the follow up experiment:

Main Effects Plot for Reacted

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Graphical output:
Mean

Data Means

95

Temp

Conc%

Point Type Corner Center

90

85

Interaction Plot for Reacted

Data Means 95
Temp 170 180 190 Point Ty pe C orner C enter C orner

80

75 170 180 190 2 3 4

90

85

Mean

80

Cube Plot (data means) for Reacted

Centerpoint Factorial Point

75
4

73

79

70 2 3 Conc% 4

Conc%

94

75 2 170 Temp

81 190

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Assessing Power: Design:

2 x 2, 1 replicate,
2 center points. Variance (MSE) = 1.28 St Dev = 1.131

Size of effect: A change of 3% in reacted substrate.

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Power Curve for 2-Level Factorial Design
1.0
Reps, Ctr Pts Per Blk 1, 2
A ssumptions A lpha 0.05 S tDev 1.131 # F actors 2 # C orner P ts 4 # Blocks none # Terms O mitted 0 Term Included In M odel C enter P oints Yes

0.8

0.6

Power

0.4

0.2

0.0

-3

-2

-1

0 Effect

This design has low power (0.165).

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Conclusions: A quadratic effect on catalytic reaction due to temperature and concentration is present. This design has low power, not the best choice. A better design would include 2 replicates, but would require 12 runs (assuming 2 center points per replicate) rather than 6.

Additional consideration: Consider using response surface methodology to model the curvature.