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Lab Test Method Validation Protocol for Laminated Films

Date:

01/06/12

Test Method:

This test method study includes 4 different tests summarized


in the table below:

Test Type
Test Instrument
National/Fed
STD #

Puncture
Instron
(100lb)

Tensile
Instron
(100lb)

Impact
(Spencer)
Elmendorf
(6400g)

Tear
Elmendorf
(200g)

FTMS-101C

D-882

D-3420

D-1922

Instrument Model and Make:


a) Instron Model 4411 MFMD007
b) Thwing Albert Pendulum/Elmendorf MMIS052
c) Dumb Bell Die Tear Sample Cutter RK-N7003CA-91W
c) JDC Precision Sample Cutter Model 1-10 (For Tensile
samples)
d) Mitutoyo Digital Micrometer IDC-112DEB (To determine
film gauge)
* Test equipments are regularly calibrated; calibration log reflects dates and calibration
periods.

Detail of Study:
Material:

Polyester/Polyethylene Laminated Film

Sample size:

3 Trials of 10 samples per tester for each test. n = 30 (90


total per test -3 testers x 30 samples each)

Purpose:
The purpose of this study is to validate puncture, tensile, impact and tear test methods
used to determine mechanical properties of packaging products at the R&D Lab.
Test Methods:
The 4 tests involved in this study are: Puncture, Impact, Tensile, and Tear strength. Due
to the nature of the tests (destructive) meaning each sample will be destroyed to obtain
the measurement reading. Therefore it is important to note that an important
assumption is made. The assumption is that the samples will be very similar in physical
characteristics (homogenous) since they are from the same work order (same film roll).
Since it is not possible for the testers to measure exact parts, a nested gage R&R study
will be conducted.
Also Anova analysis of means will be conducted to further investigate mean variability
between the different testers for each of the tests.
Puncture Test:
Test will be conducted in accordance to Federal Test Method STD. NO. 101C and Company
ABCs internal work instruction RWI-0242 (Instron 4411). Note that the 100lb Load will be

Page 1/19

used to conduct this test. Samples are cut into 2 inch strips using metal template and
razor blade.
Data for this test will be recorded automatically by Instrons software.
Tensile Strength Test:
Test will be conducted in accordance to ASTM Designation D-882 and Company ABCs
internal work instruction RWI-0242 (Instron 4411). Samples will be taken in MD direction
only for the purpose of this study. a 11.5 x 9 Metal template will be used to cut sheets
from film then use JDC sample cutter to cut samples measuring 1 inch in width and about
6 inches in length. It is critical to this test that the samples edges are free of any nicks.
Any nicks on the edge of the sample can cause an early tear and potentially skew the
results of the tensile test. One hundred pound Instron load will be used for this test.
The drawing on the right represents the sampling landscape cut from a sheet of RLA-069.
The drawing only shows the samples used for trial 1, subsequent trials will follow the
same cutting pattern utilizing additional film sheets. Data for this test will be recorded
automatically by Instrons software.
Note: Instron method 26 will be used (compression mode 00 - 12in/m).
Impact Testing (Spencer):
Impact testing method will be carried out in accordance with ASTM Designation D-3420
and Company ABCs internal work instruction RWI-0239 (Spencer Impact Test). The
Thwing Albert Pendulum/Elmendorf apparatus (using 6400g Pendulum) will be used to
conduct this test. A 4x4 metal template and a sharp cutter will be used to cut the
samples for this test. Test data will be recorded on form RFCD-0419.
Tear Testing:
Tear testing method will be carried out in accordance with ASTM Designation D-1922 and
Company ABCs internal work instruction RWI-0991 (Elmendorf Tear Propagation). The
Thwing Albert Pendulum/Elmendorf apparatus (using 200g Pendulum) will be used to
conduct this test. A spring loaded Dumb Bell die Cutter will be utilized to cut the
samples. This cutter produces samples with dimensions adhering to the requirements
found in the ASTM D-1922. Test data will be recorded on form RFCD-0419.
Data Analysis:
As mentioned above the data produced in this study will be analyzed by Anova analysis
of means and a nested gage R&R study. The data analysis will be conducted using
Minitab and the results will be interpreted in the summary and conclusion. The aim of the
study is to determine validity of the test methods as interpreted by the selected
measurement systems.

Page 2 of 19

Lab Test Method Validation Data and Results Analysis


Introduction:
Test method validation was carried out according to above protocol for Puncture, Tensile,
Impact, and tear. Test method results were analyzed in Minitab software accross 3 testers
testing 30 samples for each test (3 trials of 10 samples per tester per test). Two types of
statistical data analysis has been used for each of the tests, Anova analysis of means as
well as Gage R&R were selected to investigate the validatity of the test methods.
Puncture Testing Results:
Selected puncture test for this study is Company ABCs internal work instruction RWI0242 (Instron 4411) which is based on Federal Test Method STD. NO. 101C). Three Testers
tested 30 samples each across 3 trials using Instron. The Instron automatically logs test
values, the recorded values represents maximum load force in pounds the sample
withstands up to the point of puncturing.
Instron Crosshead speed was set to 20 in/min using a 100 lbf load unit. The Puncture
probe selected for this testing is 1/8 radius which is listed in the Federal Test Method Std
101C.
Test Data:
Sample #

Tester 1

Tester 2

Tester 3

13.92

14.23

14.88

14.22

12.93

14.71

11.81

14.09

13.37

14.45

14.38

14.23

14.53

12.59

11.73

13.74

12.64

14.3

14.86

12.91

14.15

14.29

14.84

12.69

14.61

13.32

13.49

10

13.33

13.22

14.25

11

14.35

13.94

14.15

12

13.95

14.14

14.76

13

14.01

14.44

13.25

14

13.7

12.46

14.79

15

14.32

13.71

13.81

16

11.75

14.55

14.95

17

14.52

13.26

12.72

18

13.05

13.6

13.59

19

14.05

14.1

14.18

20

13.57

14.09

13.55

21

13.45

14.33

13.99

22

14.67

14.15

13.45

23

13.69

13.23

14.37

24

13.77

12.64

13.41

25

13.35

12.71

12.98

26

13.21

13.86

13.15

27

11.88

11.98

13.93

28

14.37

13.85

13.19

29

14.56

13.52

13.01

30

13.61

10.59

13.43

Mean

13.79

13.48

13.75

0.82

0.91

0.75

Std. Dev

Puncture Resistance Test Gage R&R:


Page 3 of 19

Gage R&R (Nested) for Puncture lb/ f


Components of Variation

Puncture lb/ f By part set ( op )

100

% Contribution

14

Percent

% Study Var

50

12
10

Gage R&R

Repeat

Reprod

part set

Part-to-Part

1 2 3 4 5 6 7 8 9 10

1 2 3 4 5 6 7 8 9 10

1 2 3 4 5 6 7 8 9 10

op

R Chart by op
1

Sample Range

Puncture lb/ f by op

3
UCL=3.462

14

_
R=1.345

12

LCL=0
1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 1 0

10

part set

Sample Mean

Xbar Chart by op
1

15

2
op

UCL=15.046
__
X=13.670

14
13

LCL=12.295
1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 1 0

part set

Gage R&R Study - Nested ANOVA


Gage R&R (Nested) for Puncture lb/f
Source

DF

SS

MS

1.7106

0.855324

1.09376

0.349

part set (op)

27

21.1141

0.782005

1.21495

0.261

Repeatability

60

38.6192

0.643653

Total

89

61.4440

op

Gage R&R
%Contribution
Source

VarComp

(of VarComp)

0.646097

93.34

Repeatability

0.643653

92.98

Reproducibility

0.002444

0.35

Part-To-Part

0.046117

6.66

Total Variation

0.692215

100.00

Total Gage R&R

Study Var
Source
Total Gage R&R

%Study Var

StdDev (SD)

(5.15 * SD)

(%SV)

0.803802

4.13958

96.61

Repeatability

0.802280

4.13174

96.43

Reproducibility

0.049437

0.25460

5.94

Part-To-Part

0.214749

1.10596

25.81

Total Variation

0.831994

4.28477

100.00

Page 4 of 19

According to minitab gage R&R results, repeatablity was the most significant source of
variation. This is understandable considering the destrucutive nature of this test and
performance variation inherent in the laminated film.

Puncture Resistance, Anova analysis of means:


Before conducting anova analysis of the means, a normality test must take place.

Probability Plot of Puncture lb/ f


Normal
99.9

Mean
StDev
N
KS
P-Value

99

Percent

95
90

13.67
0.8309
90
0.085
0.110

80
70
60
50
40
30
20
10
5
1
0.1

10

11

12

13
14
Puncture lb/ f

15

16

17

Hence the P value is greater than 0.05 then one must conclude that the data is normal
and can proceed with anova anlysis of the means.
Below are the results from Minitab for executing a One way Anova anlysis on the puncture
data accross 3 testers to determine if there is a statistical difference amongst the means.

Page 5 of 19

The following is a graphical representation the results of Anova analysis of the means
amongsts all 3 testers.

One-Way Normal ANOM for Puncture lb/ f


Alpha = 0.05
14.1
14.0

13.9655

13.9

Mean

13.8
13.7

13.6704

13.6
13.5
13.4

13.3754

13.3
1

2
op

One-way ANOVA: Puncture lb/f versus op


Source
op
Error
Total

DF
2
87
89

S = 0.8286

SS
1.711
59.733
61.444

MS
0.855
0.687

R-Sq = 2.78%

F
1.25

P
0.293

R-Sq(adj) = 0.55%

The results above show a P value of 0.293. Since P value is greater than 0.05 then there
is a 95% chance that there is no statistically significant difference amongst the means
between all 3 testers. This result validates the test method results among all 3 testers
and concludes that the method is reliable and the variation is inherted from the material.

Tensile Strength Test Results:

Page 6 of 19

Tensile testing was carried out according to Company ABCs internal work instruction RWI0242 (Instron 4411) , which is based on ASTM method D882. Three Testers tested 30
samples each across 3 trials using the Instron. The Instron automatically logs test values
that represent the load force in pounds the sample can withstand up to break.
Instron Crosshead speed was set to 12 in/min using a 100 lbf load unit.
Raw Test Data:
Tensile Results
Sample #

Mean
Std. Dev

Tester 1

Tester 2

Tester 3

16.84

16.26

16.66

17.65

14.57*

18.07

18.74

14.02*

19.19

18.15

17.48

17.71

18.9

11.51*

17.61

17.82

13.59*

14.92*

14.25*

13.7

19.46

11.73*

17.62

18.99
18.75

17.56

17.12

10

19.02

13.63*

18.29

11

15.2*

16.79

14.05*

12

18.89

18.11

17.95

13

16.19

17.27

16.28

14

14.22*

17.77

18.58

15

18.59

18.95

19.01

16

18.2

13.01*

10.9*

17

14.79*

14.42

18.66

18

18.62

18.22

17.35

19

18.43

18.76

14.86*

20

15

19

18.42

21

14.23*

18.97

19.45

22

14.23*

18.17

18.76

23

15.57

17.06

17.3

24

15.75

18.08

16.56

25

13.69

18.15

17.99

26

18.83

17.47

17.22

27

14.59*

17.44

13.67*

28

18

17.78

19.33

29

14.75

17.68

18.39

30

14.32*

15.73

14.92*

16.43

16.61

17.31

2.07

2.06

2.03

Tensile Strength Gage R&R:

Page 7 of 19

Gage R&R (Nested) for Tensile lb/ f


Components of Variation

Tensile lb/ f By part set ( op )

100

20

% Contribution

Percent

% Study Var

15

50

10

Gage R&R

Repeat

Reprod

part set

Part-to-Part

1 2 3 4 5 6 7 8 9 10

1 2 3 4 5 6 7 8 9 10

1 2 3 4 5 6 7 8 9 10

op

R Chart by op
Sample Range

10

Tensile lb/ f by op

3
UCL=8.91

20

_
R=3.46

15

LCL=0
1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 1 0

10

part set

Xbar Chart by op
Sample Mean

20.0

UCL=20.323

17.5

__
X=16.782

2
op

15.0
LCL=13.241
1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 1 0

part set

Gage R&R Study - Nested ANOVA


Gage R&R (Nested) for Tensile lb/f
Source

DF

SS

MS

13.064

6.53211

1.75612

0.192

part set (op)

27

100.430

3.71962

0.83799

0.687

Repeatability

60

266.323

4.43872

Total

89

379.817

op

Gage R&R
%Contribution
Source

VarComp

(of VarComp)

Total Gage R&R

4.53247

100.00

Repeatability

4.43872

97.93

Reproducibility

0.09375

2.07

Part-To-Part

0.00000

0.00

Total Variation

4.53247

100.00

Study Var

%Study Var

StdDev (SD)

(5.15 * SD)

(%SV)

2.12896

10.9641

100.00

Repeatability

2.10683

10.8502

98.96

Reproducibility

0.30619

1.5769

14.38

Part-To-Part

0.00000

0.0000

0.00

Total Variation

2.12896

10.9641

100.00

Source
Total Gage R&R

Page 8 of 19

Gage R&R report indicates that the main source of variation is repeatability. Similar to
puncture test method validation, the data was further analysed using Anova analysis of
the means.
Tensile Strenth Anova analysis of means:
First a normality test is conducted. Following ASTMs D882 section 4.5s direction,
abnormal data points were removed from the analysis. Section 4.5 states Materials that
fail by tearing give anomalous data which cannot be compared with those from normal
failure.

Probability Plot of R - Tensile (lb/ f)


Normal
99.9

Mean
StDev
N
KS
P-Value

99

Percent

95
90

17.85
1.060
66
0.085
>0.150

80
70
60
50
40
30
20
10
5
1
0.1

14

15

16

17
18
19
R - Tensile (lb/ f)

20

21

22

Since the P value is greater than 0.05 therefore the data is normal and anova anlysis of
the means is pursued.

Page 9 of 19

One-Way Normal ANOM for R - Tensile lb/ f


Alpha = 0.05

18.4
18.263

18.2

Mean

18.0
17.846

17.8
17.6

17.428

17.4
17.2
1

2
op

One-way ANOVA: R - Tensile lb/f versus op


Source
op
Error
Total

DF
2
63
65

S = 1.046

SS
4.03
68.96
72.99

MS
2.01
1.09

R-Sq = 5.52%

F
1.84

P
0.167

R-Sq(adj) = 2.52%

The results above show a P value of 0.167. Since P value is greater than 0.05 then there
is a 95% chance that there is no statistically significant difference. amongst the means
between all 3 testers.

Page 10 of 19

Spencer Impact Test Results:


Selected Impact test methos is Company ABCs internal work instruction RWI-0239,
which is based on ASTM method D-3420. Three Testers tested 30 samples each across 3
trials using the 6400g Thwing Albert Pendulum unit. Test data results were divided by
100 and multiplied by a factor of 5.4. This is in accordance with ASTMs D-3420 Impact
testing procedure, the data results are in Jewel units.
Test Data:
Spencer Impact Results
Sample #

Tester 1

Tester 2

Tester 3

1.836

2.376

2.7

2.268

2.106

2.43

2.052

2.592

2.16

1.512

2.268

1.89

1.998

1.836

2.052

2.322

2.322

2.97

2.808

2.106

2.052

2.754

2.646

2.16

2.214

1.944

2.322

10

2.43

1.89

2.214

11

2.376

2.106

2.268

12

2.322

1.998

2.268

13

2.214

2.322

2.322

14

2.214

1.944

2.538

15

1.836

2.322

2.538

16

2.052

2.16

1.998

17

2.43

1.944

2.106

18

2.538

2.43

2.322

19

1.836

2.268

1.89

20

1.674

2.322

2.484

21

1.62

2.484

2.052

22

2.916

2.16

2.43

23

2.646

2.16

1.998

24

2.484

2.214

2.268

25

2.322

1.89

2.43

26

2.052

2.43

2.484

27

3.132

2.16

1.782

28

1.944

2.106

2.16

29

1.674

2.322

1.89

30

1.998

2.376

2.16

Mean

2.22

2.21

2.24

Std. Dev

0.40

0.21

0.26

Spencer Impact Gage R&R test Results:

Page 11 of 19

Gage R&R (Nested) for Spencer J


Components of Variation

Spencer J By part set ( op )

100

% Contribution

3.2

Percent

% Study Var

2.4

50

1.6
Gage R&R

Repeat

Reprod

part set

Part-to-Part

1 2 3 4 5 6 7 8 9 10

1 2 3 4 5 6 7 8 9 10

1 2 3 4 5 6 7 8 9 10

op

Sample Range

R Chart by op
1

Spencer J by op

UCL=1.260

3.2

_
R=0.490

2.4

1.0
0.5
0.0

LCL=0
1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 1 0

1.6

part set

Sample Mean

Xbar Chart by op
2.8

2
op

3
UCL=2.723
__
X=2.222

2.4
2.0

LCL=1.722
1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 1 0

part set

Gage R&R Study - Nested ANOVA


Gage R&R (Nested) for Spencer J
Source
op
part set (op)
Repeatability
Total

DF
2
27
60
89

SS
0.02339
3.25562
4.65199
7.93100

MS
0.011696
0.120578
0.077533

F
0.09700
1.55518

P
0.908
0.079

Gage R&R
%Contribution
(of VarComp)
84.38
84.38
0.00
15.62
100.00

Source
Total Gage R&R
Repeatability
Reproducibility
Part-To-Part
Total Variation

VarComp
0.0775332
0.0775332
0.0000000
0.0143484
0.0918816

Source
Total Gage R&R
Repeatability
Reproducibility
Part-To-Part
Total Variation

StdDev (SD)
0.278448
0.278448
0.000000
0.119785
0.303120

Study Var
(5.15 * SD)
1.43401
1.43401
0.00000
0.61689
1.56107

%Study Var
(%SV)
91.86
91.86
0.00
39.52
100.00

Page 12 of 19

Looking at the Gage R&R results, the main source of variability is repeatability. Therefore,
additional analysis will be conducted to investigate variability amongst the testers via
Anova analysis of means.
Spencer Impact, Anova analysis of means:
First a normality test will be conducted.

Probability Plot of Spencer (J )


Normal
99.9

Mean
StDev
N
AD
P-Value

99

Percent

95
90

2.222
0.2985
90
0.389
0.379

80
70
60
50
40
30
20
10
5
1
0.1

1.5

2.0
2.5
Spencer (J)

3.0

Based on a P value of 0.379, which is greater than P=0.05, the data is normal and
therefore Anova Analysis of Means is pursued.

Page 13 of 19

The following is a graphical representation of the Anova analysis of means:

One-Way Normal ANOM for Spencer (J )


Alpha = 0.05

2.35
2.3298
2.30

Mean

2.25
2.2224
2.20

2.15
2.1150

2.10
1

2
op

One-way ANOVA: Spencer J versus op


Source
op
Error
Total

DF
2
87
89

S = 0.3015

SS
0.0234
7.9076
7.9310

MS
0.0117
0.0909

R-Sq = 0.29%

F
0.13

P
0.879

R-Sq(adj) = 0.00%

Since P value is 0.879, which is greater than P=0.05, it is concluded that there is a 95%
chance that there is no statistical difference between all 3 testers and that the test
method is valid and consistent.

Elmendorf Tear Test Results:

Page 14 of 19

Test method used for Elmendorf tear test validation is Company ABCs internal work
instruction RWI-0991, which is based on ASTM method D-1922. Three Testers tested 30
samples each across 3 trials using the 200g Thwing Albert Pendulum unit. The 200 gram
unit was picked because it provides the most accurate reading for the film tested.
According to ASTM, test values are multiplied by 2 since the 200gram arm was used.
Test data:
Tear Results
Sample #

Gage R&R (Nested) for Tear G


Components of Variation

32

36

38

34

36

38

34

36

38

32

34

30

36

38

30

32

34

30

30

34

30

38

40

30

32

34

10

32

30

34

11

28

30

32

12

32

34

30

13

32

36

28

14

30

36

32

15

28

32

40

16

34

32

34

17

34

32

36

18

34

38

32

19

32

30

36

20

32

32

32

21

32

36

36

22

38

32

36

23

38

32

28

24

32

34

30

25

36

32

30

26

38

32

32

27

38

30

34

36

32

34

38

30

33.53

33.07
30

33.60

3.47

2.45
part set

3.25

% Study Var

30

Gage R&R

Repeat

Reprod

28

Tear G By part set ( op )

32

40

% Contribution

32

35

36

Mean
0

Tester 3

40

29
50

Tester 2

28

100
Percent

Tester 1

Std. Dev

Part-to-Part

op

Sample Range

R Chart by op
1

Tear G by op
UCL=13.73

40

_
R=5.33

35

LCL=0

10

part set R&R:


Tear Strength Gauge

Sample Mean

Xbar Chart by op
40

30
2
op

3
UCL=38.81
__
X=33.36

35
30

LCL=27.90
part set

Page 15 of 19

Gage R&R Study - Nested ANOVA


Gage R&R (Nested) for Tear (g)
Source
op
part set (op)
Repeatability
Total

DF
2
27
60
89

SS
3.822
218.800
608.000
830.622

MS
1.9111
8.1037
10.1333

Source
Total Gage R&R
Repeatability
Reproducibility
Part-To-Part
Total Variation

VarComp
10.1333
10.1333
0.0000
0.0000
10.1333

Source
Total Gage R&R
Repeatability
Reproducibility
Part-To-Part

StdDev (SD)
3.18329
3.18329
0.00000
0.00000

F
0.235832
0.799708

P
0.792
0.734

Gage R&R
%Contribution
(of VarComp)
100.00
100.00
0.00
0.00
100.00
Study Var
(5.15 * SD)
16.3939
16.3939
0.0000
0.0000

%Study Var
(%SV)
100.00
100.00
0.00
0.00

Looking at the Gage R&R results, repeatability is the only contributor to the variation.
Next step is to conduct normality test on the tear data to investigate further differences
among the means of the testers.

Page 16 of 19

Tear Strength, Anova analysis of means:

Probability Plot of Tear (g)


Normal
99.9

Mean
StDev
N
RJ
P-Value

99

Percent

95
90

33.36
3.055
90
0.993
>0.100

80
70
60
50
40
30
20
10
5
1
0.1

25

30

35
Tear (g)

40

45

The P value is equal to 0.100, which is greater than 0.05, this is an indication that the
data assumes a normal distribution with a confidence interval of 95%. The next step is to
conduct an Anova anlysis of the means to determine if there is a statistical difference
between the means.

Page 17 of 19

One-Way Normal ANOM for Tear (g)


Alpha = 0.05
35.0
34.5

34.453

Mean

34.0
33.5

33.356

33.0
32.5
32.258
32.0
1

2
op

The graphical representation demonstrates clearly the closeness of the means. Below is
Anova analysis of the means across all 3 testers.

One-way ANOVA: Tear (g) versus op


Source
op
Error
Total

DF
2
87
89

S = 3.083

SS
3.82
826.80
830.62

MS
1.91
9.50

R-Sq = 0.46%

F
0.20

P
0.818

R-Sq(adj) = 0.00%

With a P value of 0.818, which is greater than P=0.05, it is concluded that there is a 95%
chance of no statistical difference between all 3 testers and therefore the test method is
acceptable.

Page 18 of 19

Final Conclusion:
Test methods selected for validation study are utilized to determine physical properties of
laminated film; Puncture, Tensile, Impact, and Tear. The test methods are based on ASTM
and Federal standards interpreted into Company ABC internal procedures as referenced
above.
Output data from all four test runs was analyzed in Minitab using Anova means analysis
and gage R&R.
1. Due to material variability and the destructive nature of the tests it was not
expected to attain acceptable Gage R&R results.
2. Test run data was further analyzed to evaluate statistical variation by comparing
testers data distribution using Anova Analysis of Means. In all 4 test runs the
results pointed to the same conclusion; the means of all the testers results were
statistically similar. Therefore it is concluded that the testers and testing
equipment are capable of producing reliable results and that the main source of
variation is inherent in product and applied manufacturing processes.

Page 19 of 19