Test Method Validation Portfolio... · For the cross-hair and stent test method validation a Gage R&R study will be performed. A Gage R&R study is a test that evaluates repeatability

Test Method Validation

Christian Martinez-Carranza

Experiment performed on 10/08/10

Experiment Due on 10/20/10

Lab Friday 3 – 545pm

Professor Maryam Mobed-Miremadi

Date Submitted: 10/20/10

Grade _______________

1

Objectives

The objective is to gain experience in test method validation and to identify sources of variability in a set of measurements using Gage R&R. The second objective is to calculate the process capability for a given test.

Theory

Test method validation is used to gather evidence that a given test procedure will consistently produce results that will meet pre-determined specifications and quality targets. . According to the non-governmental standards-setting agency, the United States Pharmacopeia (USP), there are eight guidelines need to be tested for a test method validation. The guidelines are:

1] Accuracy; how close a measured test value is to the true value.

2] Precision; how consistently a measurement can be reproduced.

3] Specificity; the false positive rate of the test. A FPR is how often a measured result is considered true when the result is false.

4] Limit of quantitation; the smallest quantitation of an assay that can be made with acceptable precision and accuracy; an assay is an analysis of the composition of some substance,

5] Limit of detection; the lowest quantifiable concentration level that is statistically different from a blank sample.

6] Ruggedness; examines multiple factors that might affect the test method and determines which factor will affect the test method the greatest. Ruggedness is used to develop a standard operating procedure that will minimize the factors that will affect the robustness of a test method.

7] Robustness; the reproducibility of the test method under different conditions and in different laboratories and/or factories. The test method is considered robust if under the different conditions no unexpected results occur; the results should be consistent throughout the different conditions for a test method to be considered robust.

8] Linearity; the variance of the slope of measured test data is compared to a regression line that is calculated from the test results of a sample that was measured in a given target range.

a. Range; the upper standard limit and the lower standard limit.

For the cross-hair and stent test method validation a Gage R&R study will be performed. A Gage R&R study is a test that evaluates repeatability and reproducibility. Gage repeatability is the variation in test results from a single operator measuring the same specimen multiple times; machine variation Gage reproducibility is the variation in test results from several operators measuring the same specimen multiple times; operator-to-operator variation. A Gage R&R study is used to determine the amount of measurement variability present in the measurement system. This study can determine whether the variability is due to operator or instrument error.

2

Figure 1: Gage R&R variability from the true value

For multiple operators the Gage R&R Crossed method is used. This Gage study can be performed in two different ways, the X-bar and R, or ANOVA. The X-bar and R method simplifies the overall variation into three categories which are specimen-to-specimen, repeatability, and reproducibility. The ANOVA method is more in-depth and breaks down reproducibility into its operator, and operator by specimen, components. The ANOVA method has greater accuracy than the X-bar and R method because it accounts for the operator by specimen interaction.

Figure 2: Gage R&R Crossed method

3

Figure 3: Possible errors a Gage R&R study can reveal

Process capability is used to determine if a given process is meeting the given lower and upper specification limits. The capability of a process is analyzed by comparing the width the process variation to the lower standard limit (LSL) and upper standard limit (USL) boundaries. Before a process capability analysis can be performed a normality test must be performed to ensure that the data is normally distributed. Unlike a Gage R&R in which the distribution of the data does not need to be normal because a Gage R&R is used to determine variability in the data; variability of the data is used to determine whether the error is caused by a machine or an operator. If the data is non-normal for the capability study then it can be normalized by a Johnson Transformation or Weibull capability study can be performed. The Weibull capability study will calculate a process performance (Ppk) and not a capability performance (Cpk). Capability performance (Cpk) is a continuous process, while. Process performance (Ppk) is similar to a derivative of the process because it gives the process variation at any given point in time. Ppk is useful to determine if a process will be capable (Cpk) if process conditions could be maintained and kept stable. Ppk is also useful in determining if continuous improvement of the process has had an effect on the process.

Figure 4: Highly Capable Process: The process variation is normally distributed and fits comfortably within the LSL and USL. Specifications can be tightened in this situation.

4

Figure 5: Capable Process: The process variation is normally distributed and barely fits within the LSL and USL. Process must be carefully monitored to ensure the process stays within the specification limits.

Figure 6: Non-Capable Process: The process variation is normally distributed and doesn’t fit within the LSL and USL. The process must me refined in order to meet the specifications.

Equipment

Minitab 15.0 & 16.0

o Computer Software

o Used Minitab 15.0 on: 10/15/10

o Used Minitab 16.0 on: 10/18-19/10

Nikkon Epephot

o Brightfield/Darkfield Microscope

o Model: FX-35WA

o SVMS ID # 00488

o SJSU ID # 211771

o Alamaden OP Technology

Collimation Check

5

Equipment

S/N: 211770

Date: 5/1998

Due: 5/1999

Stereomicroscope

o 3D Digital Video microscope

o 12.5x for all tests

o Caltex Systems

o ID # VZM-200

o SJSU ID # 30137

o Caltexsci.com

o 18772CALTEX

Materials

Stent and Microcapsule samples

Procedure

1) Have each operator measure 15 different parts of the stent sample using the Stereomicroscope.

a. Repeat step 1: Should obtain a total of 30 part measurements from each operator.

2) Measure 30 different parts of the microcapsule sample using the Stereomicroscope.

a. Repeat step 2 for Petri dish 1, 2 and 3: Should obtain a total of 90 part measurements from all microcapsule samples.

3) Have each operator measure 15 different parts of the stent sample using the Brightfield/Darkfield microscope.

a. Repeat step 3: Should obtain a total of 30 part measurements from each operator.

Data Summary

See Appendix

6

Discussion

The stent gage R&R had a repeatability variance of 18.03%, reproducibility variance of 79.03%, operator variance of 69.53% and a part-to-part variance of 2.94%. The gage R&R study shows that there is large variance in the operator data.

The cross-hair stent gage R&R had a repeatability variance of 17.31%, reproducibility variance of 82.69%, operator variance of 70.91% and a part-to-part variance of 0%. The gage R&R study shows that there is large variance in the operator data.

The microcapsule normality test for Petri dish 1 had a P-value <0.005, which is below the 95% confidence interval required for a data set to be considered normal; the data set was non-normal. The microcapsule normality test for Petri dish 2 had a P-value = 0.283 > 0.05, which is above the 95% confidence interval required for a data set to be considered normal. The microcapsule normality test for Petri dish 3 had a P-value = 0.815 > 0.05, which is above the 95% confidence interval required for a data set to be considered normal.

The Ppk of Petri dish 1 is -0.36, Pp is 0.47 and the non-normal data did not stay within the LSL and USL. Petri 1 did not meet the targets of 300, 500 and 2000 microns. The Cpk of Petri dish 2 is 2.91, the CP is 9.77 and the normal data did stay within the LSL and USL. Petri 2 did not meet the targets of 300, 500 and 2000 microns. The Cpk of Petri dish 3 is 3.43, the CP is 16.34 and the normal data did stay within the LSL and USL. Petri 3 did not meet the targets of 300, 500 and 2000 microns.

Conclusion

The stent gage R&R study shows that there is large operator-to-operator measurement variance signifying that the error is caused by the operator. The variance in the data may be due to operator inexperience or lack of standard measuring procedures. The variance part-to-part is 2.94% and is very low, which means that an operator’s individual data correlated, but did not correlate when compared to the data of the other operators. This result further confirms that the error is caused by an operator and not the machine.

The cross-hair stent gage R&R study has similar results to that of the stent gage R&R. There is large variation in the operator-to-operator data, with low variation part-to-part. This result further confirms that the error is caused by the operator because the same operators performed the cross-hair stent measurements.

Out of the three Petri dishes of microcapsules only Petri dish one had non-normal data. Petri dish 1 had a negative Ppk, which means that it is a non-capable process. Petri dish 1 targets of 300 and 500 did fall within the data set, but the targets did not lie in the optimal position, which it at the max of the bell curve the targets were close to the USL. Petri dish 2 and 3 had positive Cpk and Cp, which would indicate that these are good processes. But the data range is for both was typically confined in a small area and had a lot of free space within the LSL and USL. The normal distribution of Petri 2 and 3 didn’t meet any of the targets which indicate that the process needs to be refined to meet the targets. According to the capability study this is a non-capable process and needs further refinement in order to meet the targets.

A major error occurred during the microcapsule measurements; the microcapsules were measured incorrectly because the program that was used was measuring the number of pixels across the screen and not the actual diameter of the microcapsule itself. This became apparent when the pixels were converted

7

to centimeters and the diameters of the spheres were obviously bigger than the true value. The pixel-to-micron ratio used was the quantum pixel-to-micron conversion. This isn’t the correct conversion because the ratio of microns to pixels changes depending on the computer monitor because every monitor has a different pixel count depending on its resolution. For example a monitor may be 1920 pixels by 1200 pixels, in which case if you knew the dimensions of the screen the microns per pixel ratio can be calculated. Unfortunately the dimensions and resolution of the computer monitor used were not gathered, so an accurate dimensional analysis couldn’t be made.

Bibliography

1] Huber, Ludwig. "Validation of Analytical Methods and Procedures." Lab Compliance. Web. 14 Oct. 2010. <http://www.labcompliance.com/tutorial/methods/default.aspx>.

2] "Method Validation." GMP-Quality up. Web. 18 Oct. 2010. <www.gmpqualityup.com/sample/VAL-015_sample.pdf>.

3] "ASTM E1169 -07 Standard Practices for Conducting Ruggedness Tests." ASTM International - Standards Worldwide. Web. 18 Oct. 2010. <http://www.astm.org/Standards/E1169.htm>.

4] Vander Heyden, Y., A. Nijhuis, J. Smeyers-Verbeke, B.G.M. Vandeginste, and D.L. Massart. "Guidance for Robustness/Ruggedness tests in Method Validation." Pharmaceutical Institute. Vrije University of Brussel, 27 Mar. 2006. Web. 18 Oct. 2010. <www.vub.ac.be/fabi/tutorial/guideline.pdf>.

5] "Analytical Detection Limit Guidance and Laboratory Guide for Determining Method Detection Limits." Laboratory Certification Program. Wisconsin Department of Natural Resources. Web. 18 Oct. 2010. www.dnr.state.wi.us/org/es/.../lod%20guidance%20document.pdf

6] Minitab. Vers. 16.0. State College, PA: Minitab, 2010. Computer software. 7] Scutoski, Hank, and Chander Sekar. "Introduction to Gage R&R Studies." Semiconductor Wafer Test

Workshop. Web. 18 Oct. 2010. www.swtest.org/swtw_library/1998proc/.../T1_Hank.PDF 8] "Display Resolution." Wikipedia, the Free Encyclopedia. Web. 19 Oct. 2010.

<http://en.wikipedia.org/wiki/Display_resolution>. 9] "Process Capability Analysis." Pioneer CT, TPM-Trak®, Productivity, OEE, DNC, CAM, Tool Monitoring,

Wireless, CNC, Drip Feed, Technology Solutions, Enterprise Applications. Web. 19 Oct. 2010. <http://www.pioneerct.com/whitepapers/processcapability/processcapability.html>

8

Appendix

1] TABLE 1: Microcapsule Data PD1



4] TABLE 4: Stent Data – Chris

5] TABLE 5: Stent Data – Kenny

6] TABLE 6: Stent Data – Ning

7] TABLE 7: Stent Data – Sukhdeep

8] TABLE 8: GAGE R&R Stent Study results

9] TABLE 9: Cross-Hair Data

10] TABLE 10: GAGE R&R Cross-Hair Study results

11] Figure 1: Normality Test Petri Dish 1

12] Figure 2: Normality Test Petri Dish 2

13] Figure 3: Normality Test Petri Dish 3 14] Figure 4: Capability Sixpack (Weibull) PD 1

15] Figure 5: Capability (Weibull) PD 1

16] Figure 6: Capability (Normal) PD 2

17] Figure 7: Capability (Normal) PD 3

18] Figure 8: Capability (Weibull) PD 1 @ target of 300 microns

19] Figure 9: Capability (Normal) PD 2 @ target of 300 microns


21] Figure 11: Capability (Weibulll) PD 1 @ target of 500 microns



24] Figure 14: Capability (Weibull) PD 1 @ target of 2000 microns



27] Figure 17: GAGE R&R (Crossed) for Stent

28] Figure 18: GAGE R&R (Crossed) for Stent Cross-Hair measurement

29] Figure 19: Microcapsule Images



32] Figure 22: Stent Images (Kenny)

33] Figure 24: Stent Images (Ning)

34] Figure 25: Stent Images (Sukhdeep

35] Figure 25: Stent Images (Chris)

9

TABLE 1: Microcapsule Data PD1

Microcapsule Petri Dish 1

1 Pixel = 70.7 Microns

Sample 1 (Needle Dog Practiced 9/15)

1 Micron = 0.001 mm

Run on: 10/1/2010

1 mm = 0.1 cm

All measurements in Pixels Measuring equipment: Serological Microscope

Area Mean Min Max Diameter (Pixels) Diameter (cm)

1 153432 170.68 142 202 441.990392 3.124872071

2 134908 166.666 136 201 414.4514922 2.93017205

3 101212 166.94 138 200 358.9805008 2.537992141

4 34964 165.924 134 209 210.9917195 1.491711457

5 62001 168.588 139 207 280.9662809 1.986431606

6 115850 160.354 128 214 384.0633579 2.715327941

7 20527 166.766 139 199 161.665592 1.142975735

8 71636 167.738 140 197 302.0094411 2.135206748

9 47168 167.935 137 245 245.0634745 1.732598765

10 47168 164.464 137 199 245.0634745 1.732598765

11 47168 162.258 129 192 245.0634745 1.732598765

12 45788 165.701 131 220 241.4519364 1.70706519

13 43360 170.62 142 245 234.9630075 1.661188463

14 46904 168.425 140 199 244.3767002 1.72774327

15 45802 166.579 137 217 241.4888464 1.707326144

16 62432 168.573 140 201 281.9411582 1.993323989

17 56634 170.942 144 200 268.5304094 1.898509994

18 38534 164.933 133 201 221.5016176 1.566016436

19 40272 166.01 131 196 226.4417251 1.600942996

20 107524 163.77 133 206 370.0049735 2.615935163

21 51060 169.408 130 255 254.9736264 1.802663539

22 60842 166.977 140 210 278.3278062 1.96777759

23 122714 171.848 141 207 395.2773342 2.794610753

24 46709 167.069 138 203 243.8681818 1.724148046

25 41068 165.872 134 202 228.6686524 1.616687372

26 66257 167.461 139 201 290.4495712 2.053478468

27 38414 164.769 132 195 221.1564559 1.563576143

28 79307 159.654 129 215 317.7683337 2.246622119

29 73547 162.559 130 193 306.0112105 2.163499258

30 45620 166.845 134 198 241.0085757 1.70393063

10


Microcapsule Petri Dish 2

1 Pixel = 70.7 Microns

Sample 2 (9/15)

1 Micron = 0.001 mm

Run on: 10/1/2010

1 mm = 0.1 cm

All measurements in Pixels Measuring equipment: Serological Microscope


1 40019 167.59 133 207 225.729427 1.595907049

2 34754 171.082 141 210 210.3572387 1.487225678

3 39150 169.617 138 211 223.2651541 1.578484639

4 45746 167.497 139 214 241.3412878 1.706282905

5 43912 165.34 135 203 236.4540037 1.671729806

6 38679 168.068 134 202 221.9180777 1.568960809

7 38679 170.568 140 238 221.9180777 1.568960809

8 44868 172.976 142 238 239.0140432 1.689829286

9 44100 171.633 145 209 236.9596271 1.675304564

10 59092 169.512 141 202 274.2959578 1.939272422

11 46964 168.49 138 200 244.5330714 1.728848815

12 46964 164.778 131 211 244.5330714 1.728848815

13 48304 167.683 141 199 247.9971049 1.753339531

14 32016 167.609 135 216 201.9010598 1.427440493

15 36556 170.994 141 213 215.7418494 1.525294875

16 45324 169.554 141 204 240.2255401 1.698394568

17 49092 167.971 137 209 250.0117533 1.767583096

18 46312 161.444 128 209 242.8297156 1.71680609

19 42975 162.483 130 213 233.9176572 1.653797837

20 42975 168.596 135 208 233.9176572 1.653797837

21 46656 168.823 139 214 243.7299022 1.723170408

22 48315 167.964 140 200 248.0253407 1.753539159

23 37967 168.673 140 215 219.8660652 1.554453081

24 38190 168.449 139 202 220.5108139 1.559011454

25 42450 161.839 131 199 232.4844502 1.643665063

26 49682 165.2 137 202 251.5096184 1.778173002

27 45896 163.883 134 210 241.73664 1.709078045

28 34104 162.185 127 204 208.3808105 1.47325233

29 46475 156.885 128 195 243.2566728 1.719824677

30 41020 162.959 133 201 228.5350892 1.615743081

11


Microcapsule Petri Dish 3 Sample 3 (9/20, 5/20) Run

on: 10/1/2010 All measurements in pixels

Measuring equipment: Serological Microscope


1 25930 163.978 133 201 181.7005833 1.284623124

2 30139 169.74 139 207 195.8932548 1.384965312

3 33633 172.757 143 210 206.9368656 1.46304364

4 33633 174.191 146 213 206.9368656 1.46304364

5 30067 174.044 141 219 195.6591272 1.383310029

6 29225 170.577 134 219 192.9000423 1.363803299

7 29225 165.801 140 207 192.9000423 1.363803299

8 29785 167.247 133 206 194.7394169 1.376807677

9 31250 171.124 133 214 199.4711419 1.410260973

10 30932 170.676 134 219 198.4536376 1.403067218

11 29496 173.969 141 219 193.7923483 1.370111902

12 27148 174.613 146 213 185.9190893 1.314447961

13 28887 172.311 143 204 191.7813113 1.355893871

14 32692 167.176 138 204 204.0214398 1.44243158

15 27132 172.622 141 222 185.8642944 1.314060561

16 31541 172.74 143 222 200.3977274 1.416811933

17 29370 173.111 148 218 193.3779875 1.367182372

18 27576 171.836 138 209 187.3789057 1.324768863

19 29530 170.851 139 214 193.9040082 1.370901338

20 28688 168.294 136 214 191.1195874 1.351215483

21 34588 167.952 138 206 209.8542592 1.483669613

22 28545 176.822 143 214 190.642659 1.347843599

23 28545 176.31 143 241 190.642659 1.347843599

24 30630 168.874 131 205 197.482475 1.396201098

25 32969 167.317 135 196 204.8839556 1.448529566

26 36209 167.715 137 208 214.7154663 1.518038347

27 30568 169.789 138 207 197.2825057 1.394787316

28 23584 171.351 141 209 173.2861274 1.22513292

29 25661 175.514 151 224 180.7556376 1.277942358

30 26760 170.593 138 212 184.5857275 1.305021093

12

TABLE 4: Stent Data – Chris

Stent Sample 1 Operator Chris Run On: 10/1/2010 All measurements in pixels

Equipment: Stereomicroscope at 12.5 x for all 3 trials Total

Runs Trials Area Mean Min Max Angle Length Diameter

1 1 250 142.481 128.22 197.743 11.853 248.66 17.84124

2 2 243 144.351 132.044 178.334 4.508 241.525 17.58969

3 3 246 144.104 127.299 169.147 -8.461 244.786 17.69794

4 1 249 152.931 139.315 166.796 -43.523 247.504 17.80552

5 2 243 149.467 134.963 166.301 -37.107 242.139 17.58969

6 3 230 152.138 141.241 172.505 101.065 229.087 17.11272

7 1 225 153.235 140.932 173.311 107.949 223.826 16.92569

8 2 226 153.353 139.253 168.057 107.628 224.687 16.96326

9 3 227 152.846 136.695 167.281 91.521 226.233 17.00075

10 1 229 148.781 135.483 160.883 62.873 228.479 17.07548

11 2 259 168.149 154.461 198.203 57.853 257.651 18.15954

12 3 257 165.312 147.336 209.356 55.008 256.132 18.08929

13 1 257 168.294 153.787 186.587 49.764 255.859 18.08929

14 2 255 166.921 146.098 190.862 89.775 254.113 18.01877

15 3 255 176.046 158.21 199.826 71.565 253.691 18.01877

13

TABLE 5: Stent Data – Kenny

Stent Sample 1 Operator Kenny Run On: 10/1/2010 All measurements in pixels



1 1 259 162.849 149.991 195.35 18.295 257.898 18.15954

2 2 262 159.31 146.821 186.388 27.544 261.24 18.26441

3 3 258 157.97 145.29 190.689 28.256 256.536 18.12445

4 1 262 156.945 143.934 184.276 32.354 261.321 18.26441

5 2 255 155.934 135.552 178.419 33.128 254.222 18.01877

6 3 269 151.21 136.225 167.777 -24.179 268.005 18.50679

7 1 256 149.015 126.968 171.754 -29.272 254.958 18.05407

8 2 248 153.112 138.099 169.006 -33.111 247.246 17.76973

9 3 238 159.074 145.8 178.706 -41.754 237.434 17.40779

10 1 257 152.415 134.77 167.431 27.561 256.47 18.08929

11 2 259 168.731 153.32 219.735 48.772 257.946 18.15954

12 3 259 175.346 161.694 196.556 -

133.112 257.527 18.15954

13 1 236 179.264 162.698 199.624 13.799 234.776 17.33449

14 2 234 184.211 166.373 249.497 6.394 233.452 17.26088

15 3 266 158.599 147.95 175.321 40.414 265.307 18.40331

14

TABLE 6: Stent Data – Ning

Stent Sample 1 Operator Ning Run On: 10/1/2010 All measurements in pixels



1 1 258 157.843 143.574 187.04 40.892 256.632 18.12445

2 2 257 173.023 158.24 204 51.34 256.125 18.08929

3 3 260 173.6 158.747 196.372 58.276 258.643 18.19457

4 1 245 177.992 159.98 196.324 69.334 243.68 17.66193

5 2 239 183.376 167.168 223.008 7.245 237.899 17.44432

6 3 265 157.978 144.409 172.822 49.917 264.015 18.36868

7 1 257 157.93 137.54 189.673 38.032 256.453 18.08929

8 2 252 173.688 155.206 197 62.008 251.412 17.91246

9 3 261 158.317 140.508 179.121 51.546 260.5 18.22952

10 1 261 162.232 151.286 179 42.51 260.461 18.22952

11 2 241 161.086 145.096 174.475 24.642 239.842 17.51716

12 3 261 157.137 141.599 174 46.868 260.354 18.22952

13 1 262 160.293 142.334 210.619 49.97 261.197 18.26441

14 2 250 174.404 161.806 187.333 57.458 249.11 17.84124

15 3 240 164.841 150.721 175.553 20.106 238.537 17.48078

15

TABLE 7: Stent Data – Sukhdeep

Stent Sample 1 Operator Sukhdeep Run On: 10/1/2010 All measurements in pixels



1 1 245 161.181 144.734 200.588 6.833 243.898 17.66193

2 2 238 160.834 145.614 187.625 13.627 236.848 17.40779

3 3 233 161.834 146.146 177.273 11.94 232.488 17.22396

4 1 225 159.996 144.914 183.566 10.856 223.609 16.92569

5 2 209 161.798 148.05 207.085 20.266 208.349 16.31279

6 3 202 169.053 152.984 185.803 11.757 201.175 16.03728

7 1 201 170.042 153.998 205.886 23.236 199.673 15.99754

8 2 194 165.199 145.462 208.278 28.421 193.46 15.7165

9 3 188 165.485 141.966 181.154 26.428 186.828 15.47156

10 1 195 165.028 150.844 192.427 14.323 193.606 15.75696

11 2 203 166.346 151.188 201.476 12.867 202.031 16.07693

12 3 194 174.677 152.967 201.266 31.88 193.062 15.7165

13 1 241 162.641 146.33 202.646 3.352 239.922 17.51716

14 2 187 166.387 152.459 187.837 8.653 185.711 15.43035

15 3 195 166.787 153.678 201.936 12.817 193.657 15.75696

16

TABLE 8: GAGE R&R Study results ————— 10/18/2010 11:37:35 PM ————————————————————

Welcome to Minitab, press F1 for help.

Gage R&R Study - ANOVA Method

Gage R&R for Diameter Measure

Gage Name: Gage R&R (Crossed) - Stent Date of Study: 10/2/2010

Reported By: Chris, Sukhdeep, Ning, Kenny Tolerance:

Misc: Diameter measured in pixels Two-Way ANOVA Table With Interaction Source DF SS MS F P

Trials 14 7.3622 0.5259 1.6339 0.109

Operator 3 55.3382 18.4461 57.3131 0

Trials * Operator 42 13.5176 0.3218 2.0544 0.005

Repeatability 60 9.3998 0.1567 Total 119 85.6178

Alpha to remove interaction term = 0.25 Gage R&R

Source VarComp % Contribution of VarComp Total Gage R&R 0.843396 97.06

Repeatability 0.156663 18.03 Reproducibility 0.686733 79.03 Operator 0.604141 69.53 Operator * Trials 0.082592 9.51 Part-to-Part 0.025503 2.94 Total Variation 0.868899 100

Source

StdDev (SD) Study Var (6*SD) %Study Var

Total Gage R&R 0.918366 5.51019 98.52 Repeatability 0.395806 2.37484 42.46 Reproducibility 0.828694 4.97216 88.9 Operator 0.777265 4.66359 83.38 Operator * Trials 0.287389 1.72433 30.83 Part-to-Part 0.159698 0.95819 17.13 Total Variation 0.932148 5.59289 100 Number of Distinct Categories = 1


17

TABLE 9: Cross-Hair Data

Stint I Stint Diameter based on rotations

1 crosshair is 1000 microns Part Sukhdeep Ning Kenny Chris

1 1 1.8 0.7 0.4

2 0.75 1.6 0.5 0.6

3 1.5 1 0.5 0.3

4 1.75 0.75 0.8 0.3

5 2 1.3 0.7 0.5

6 1.5 1.5 0.4 0.7

7 1.7 1 1 0.5

8 1.6 0.8 0.7 0.3

9 2 0.75 0.5 0.4

10 1.8 1.5 0.8 0.5

11 1.5 1 0.4 0.4

12 1.7 1.5 0.9 0.3

13 1.7 0.75 1 0.3

14 0.75 0.75 0.9 0.3

15 1.5 1 0.7 0.3

18

TABLE 10: GAGE R&R Cross-Hair Study results

————— 10/18/2010 11:37:35 PM ———————————————————— Welcome to Minitab, press F1 for help.

Gage R&R Study - ANOVA Method

Gage R&R forCross-Hair Measurement

Gage Name: Gage R&R (Crossed) - Cross-Hair Measurement of Stent Date of Study: 10/2/2010

Reported By: Chris, Sukhdeep, Ning, Kenny Tolerance:

Misc: Diameter measured in rotations Two-Way ANOVA Table With Interaction

Source DF SS MS F P Trials 14 0.6059 0.04328 0.3225 0.987 Operator 3 21.3589 7.11964 53.0554 0 Trials * Operator 42 5.6361 0.13419 2.3612 0.001 Repeatability 60 3.41 0.05683

Total 119 31.0109 Alpha to remove interaction term = 0.25 Gage R&R

Source VarComp % Contribution of VarComp Total Gage R&R 0.328361 100

Repeatability 0.056833 17.31 Reproducibility 0.271528 82.69 Operator 0.232848 70.91 Operator * Trials 0.03868 11.78 Part-to-Part 0 0 Total Variation 0.328361 100

Source StdDev (SD) Study Var (6*SD) %Study Var Total Gage R&R 0.573028 3.43817 100

Repeatability 0.238397 1.43038 41.6 Reproducibility 0.521083 3.1265 90.94 Operator 0.482543 2.89526 84.21 Operator * Trials 0.196671 1.18003 34.32 Part-to-Part 0 0 0 Total Variation 0.573028 3.43817 100 Number of Distinct Categories = 1


19

Figure 1: Normality Test Petri Dish 1


20


Figure 4: Capability Sixpack (Weibull) PD 1

21

Figure 5: Capability (Weibull) PD 1

Figure 6: Capability (Normal) PD 2

22

Figure 7: Capability (Normal) PD 3

Figure 8: Capability (Weibull) PD 1 @ target of 300 microns

23

Figure 9: Capability (Normal) PD 2 @ target of 300 microns


24

Figure 11: Capability (Weibulll) PD 1 @ target of 500 microns


25


Figure 14: Capability (Weibull) PD 1 @ target of 2000 microns

26



27

Figure 17: GAGE R&R (Crossed) for Stent

28

Figure 18: GAGE R&R (Crossed) for Stent Cross-Hair measurement

29

Figure 19: Microcapsule Images



30

Figure 22: Stent Images (Kenny)

Figure 23: Stent Images (Ning)

Figure 24: Stent Images (Sukhdeep)

Figure 25: Stent Images (Chris)

Documents

Test Method Validation Portfolio... · For the cross-hair and stent test method validation a Gage R&R study will be performed. A Gage R&R study is a test that evaluates repeatability