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ICRI REPORT #641 DISTRIBUTION LIST ICRI Trustees: Ben Grigg - Aarrowcast Art Boehme - Casting Solutions John Haas - Grede Holdings, LLC Scott McIntyre - John Deere John Burke - OSCO Paul Campbell - Tyco John Dailleboust - Wescast

Randall Lawton - C.A. Lawton John Hendrix - Glidewell Dick Haun - Gunite Jim O'Sullivan - Motor Castings Richard Nicholas - Quality Kevin Barron - Ward Mfg.

J.B. Brown - Bremen Rob Killips - Great Lakes John McGoldrick - Hodge Frank Headington - Neenah Robert Kersey - Rochester Mike Mroczek - Weil McLain

Technical Committee Mail list: (Not otherwise listed) Cesar Braga - Aarrowcast Brad Harris - Bremen Richard Lewis - Elyria Kurt Becker - Great Lakes Daryl Konsler - Grede-Brewton Bill Harvey - Grede-Columbiana Randy Priem - Grede Iron Mtn. Larry Carmack - Grede-St.Cloud Mike Forsha - Hodge Foundry Scott McIntyre - John Deere Mike Riabov - Neenah Chris Maness - OSCO-Jackson Tom Brower - OSCO-New Boston Greg Loving - Rochester Don Perry - Tyco Brent Black - Wescast-Wingham

Andrew Zillman - Aarrowcast Rob Christensen - C.A.Lawton James Lawrence - Elyria Tim Stefanick - Great Lakes Calvin Simon - Grede-Columbiana Chris Greene - Grede-Columbiana Dan Antonetti - Grede-Reedsburg Rob Schmidt - Grede-St. Cloud Ashley Assink - John Deere Leonard Lamb - Motor Castings Phil Kubichka - Neenah Jim Jensen - OSCO-Portsmouth Matt Nicholas - Quality Craig Sederholm - Rochester Carlos Crespo - Weil McLain Feila Yu - Wescast-TDC

Matthew Meyer - Bremen Jeff Drury - Dalton-Warsaw Brian Richey - Glidewell Randy Hunt - Grede-Brewton Jim LeCroy - Grede-Columbiana Greg Jarski - Grede-Iron Mtn. Mike Rothwell - Grede-Reedsburg Tony Clark - Gunite Ernie Timmons - John Deere Stan Hemenway - Motor Castings Keith Denny - OSCO-Jackson Jake Hackworth - OSCO-Portsmouth John Nicholas - Quality Matt Calcutt - Rochester Cheryl Cichowlaz - Weil McLain

Participants: (Not Otherwise Listed) Jim Frost - ACIPCO Lori Felber - Anderson Labs Keith Provine - Benton Dave Hiles - OSCO-New Boston

Don Denney - ACIPCO Matt Lobos - Benton Jim Cree – Grede - New Castle

Greg Mann - Anderson Labs Jeff Hall - Benton Jeff Hipple - Grede-New Castle


ICRI REPORT #641 INTERLABORATORY SPECTROMETER PROFICIENCY STUDY ROUND 32 RESULTS BY BRUCE T. BLATZER APRIL 9, 2013


ICRI Report No. 641 4/9/13

Table of Contents

Page

Discussion ........................................................................................................................... 1 Figure 1: Number of h and k Occurrences .......................................................................... 5 Silicon Chart ....................................................................................................................... 6 Silicon Graphs .................................................................................................................... 7 Manganese Chart ............................................................................................................... Manganese Graphs ............................................................................................................

8 9

Sulfur Chart ...................................................................................................................... Sulfur Graphs ...................................................................................................................

10 11

Phosphorus Chart ............................................................................................................. Phosphorus Graphs ...........................................................................................................

12 13

Chromium Chart ............................................................................................................... Chromium Graphs ............................................................................................................

14 15

Copper Chart .................................................................................................................... Copper Graphs .................................................................................................................

16 17

Tin Chart ........................................................................................................................... Tin Graphs ........................................................................................................................

18 19

Magnesium Chart ............................................................................................................ Magnesium Graphs ..........................................................................................................

20 21

Aluminum Chart .............................................................................................................. Aluminum Graphs ............................................................................................................

22 23

Cerium Chart .................................................................................................................... Cerium Graphs .................................................................................................................

24 25

Appendix I ........................................................................................................................ Appendix II ....................................................................................................................... Appendix III ......................................................................................................................

26 27 28


ICRI REPORT NO. 641 4/9/13

Interlaboratory Spectrometer Proficiency Testing Round 32 Introduction Proficiency testing is a tool that is used to measure the precision of various testing methods. In this case we have chosen the spectrometer testing method located at each participating laboratory to measure proficiency. The purpose of this testing program is to give performance feedback to each lab on an element-by-element basis at three different concentrations so that each member can make a determination of where to concentrate available resources for improvement. ASTM E691-05, Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method, is the practice being followed for all proficiency testing. Thirty three labs (spectrometers) participated in this Thirty Second round. Explanation of Testing In mid February, three standards were sent to all participating labs for testing. These standards represented three concentrations of each element of interest. Each standard was to be tested five times recording the test results on the form sent for this purpose. No extreme measures were to be made to enhance results. Elements in this thirty second round of testing were silicon, manganese, sulfur, phosphorus, chromium, copper, tin, magnesium, aluminum and cerium. Results All received test results were entered into a spreadsheet for analysis. Statistical values are presented in the tables. Data from the actual testing are presented on the enclosed graphs. The graph for each respective element follows its statistical table page. The statistics that separate chance variability from controllable factors are h and k values. The h value is a measure of reproducibility or consistency between labs. The k value is a measure of the repeatability or consistency within a lab. If a lab’s h or k values for a specific concentration of an element are higher than the test critical values (|hcrit| > 2.64 and kcrit > 1.89), there is a “statistically significant” difference between that lab’s results and the other lab’s results. These critical values are based on 95% probability limits and must not be treated as exact mathematical quantities, but as rough guides. See Appendix I for an explanation of critical values. Blanks in the tables can represent a number of conditions. The most common is no data was reported for that particular element. Another reason is where only one test result is reported for a concentration instead of five. In this case a standard deviation cannot be calculated and is therefore left blank as well as its associated k value. Generally, those labs with “statistically significant” variations should investigate and correct root causes for the differences. Even if the magnitude of one of the statistics is not quite high enough to be in the critical zone (above the absolute value of hcrit and above kcrit), investigative and corrective action should Page 1


ICRI REPORT NO. 641 4/9/13

be implemented. Corrective action should be taken especially if both h and k values are near the critical level for any element or concentration. If this situation exists it means that your lab’s results did not agree with the group nor were the results consistent within your own lab. Thirteen spectrometers or 39.4% registered zero h and k occurrences, a deterioration from the last round. 53% of the spectrometers achieved zero h and k occurrences on Round 31. Good judgement should be used when determining whether corrective action should be instituted. For instance, there may be a logical answer for your test results being consistently and significantly above or below normal operating ranges. Example: low sulfur concentrations are probably of no interest to gray iron producers, nor are high magnesium concentrations and, therefore, those elements may not be properly standardized for the ranges seen on these samples. If a calculated value of h and k is greater than its respective critical value, then a bold h or k letter is printed to the right of the offending value in the data tables. Graphs There are three graphs (low, medium and high concentrations) for each element tested. Each lab number is plotted on the x axis. Each plotted data point, on the y axis, represents an actual test result. The average for each lab’s test results is plotted slightly to the right of the actual test results. The average of the averages or interlab average for each concentration is displayed below and to the left of each graph. The actual interlab averages for the three concentrations can be found on the respective table for each element. Summary of h and k statistics Figure 1 shows a summary of the lab results in terms of number of occurrences of h and k greater than the critical values. If there is a bar next to your lab number, a serious study of the root causes with subsequent corrective action should be undertaken. If your lab does not have a bar next to it, a closer look at the h and k values could very well show that improvement can be made. There is no hard rule, but we think that reasonable targets of h values should be less than the absolute value of 1 and less than 1 for k values. Element Consistency The table below shows a breakdown by element of the number of critical h and k value results. Low values and especially zero are more desirable. This table indicates there is much work to be done in developing more accurate curves but operator-to-operator variation within individual laboratories remains the larger issue needing attention and improvement. Round 32 Elements h above critical k above critical Sum of h & k

Si Mn 2 2

S 3

P 4

Cr Cu Sn Mg Al Ce 2 2 5 2 3 3

32%

7

6

5

10

6

7

4

4

7

4

68%

9

8

8

14

8

9

9

6

10

7

88

Page 2


ICRI REPORT NO. 641 4/9/13

Comments by element Silicon Two spectrometers exceeded the hcrit. value on low and medium concentration samples for a total of two. There were seven occurrences above the kcrit value, five from two spectrometers. Manganese Two spectrometers exceeded the hcrit value on the low and medium concentration samples. There were six occurrences above the kcrit value, five from two spectrometers. Sulfur One spectrometer exceeded the hcrit value on the low, medium and high concentration samples. Consistency within labs was a larger problem with five occurrences above the kcrit value, two from one spectrometer. The most variation occurred on the average low concentration. Phosphorus Three spectrometers exceeded the hcrit value on this element. Within lab variation was higher with ten occurrences above the kcrit value. Chromium Two spectrometers exceeded the hcrit value with two occurrences. Five labs exceeded the kcrit value with six occurrences above the kcrit value. Copper Two spectrometers exceeded the hcrit value on all low and high concentration samples. Six spectrometers exceeded the krit value with seven occurrences above the kcrit value. Tin Three spectrometers exceeded the hcrit value with five occurrences. Three spectrometers exceeded the krit value with four occurrences above the kcrit value. One spectrometer skewed the average low concentration and resulted in a high coefficient of variation for this parameter. Magnesium Two spectrometers exceeded the hcrit value. There were four occurrences above the krit value. Aluminum Two spectrometers exceeded the hcrit value with three occurrences. Five spectrometers exceeded the kcrit value on seven samples. Page 3


ICRI REPORT NO. 641 4/9/13

Cerium Twenty one spectrometers reported cerium concentrations. There were three occurrences above the hcrit value, all from one spectrometer. There were four occurrences that exceeded the kcrit value, three from one spectrometer and one from another spectrometer. Cerium is an element that few labs seem to have good certified samples for calibration. Conclusion: The totals of h and k values exceeding their respective critical levels show that a decline occurred since this same testing was performed one year ago and from six months ago. Additional work is needed if proficiency is to continually improve. Most of the decline came in increasing variation within the labs. We recommend a continuation of work on reducing all variation, within the labs and from lab to lab. This may require more training on proper maintenance and operation of the spectrometer for your operators and managers. If anyone is interested in a class on principles and operation of spectrometers, please let us know. Bruce Blatzer

Page 4


INTERLAB SPECTROMETER TESTING

ICRI REPORT NO. 641 4/9/13

FIGURE 1

Number of h and k Occurrences 0

1

2

3

4

5

6

7

8

9 10 11 12 13 14 15

Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

k's h's

Average = 2.7

Zero is the goal

Page 5


TABLE 1

ICRI REPORT NO 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

SILICON

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

Target Interlab Avg Std Dev of Avg Coef of variation

AVERAGE Low Si Med Si High Si 1.54 1.66 2.42 1.61 1.71 2.38 1.57 1.67 2.34 1.56 1.63 2.32 1.61 2.33 1.54 1.63 2.30 1.54 1.66 2.39 1.35 1.70 2.18 1.59 1.67 2.38 1.80 1.74 2.43 1.42 1.85 2.32 1.64 1.63 2.30 1.72 1.65 2.31 1.75 1.66 2.32 1.54 1.69 2.41 1.59 1.69 2.38 1.48 1.60 2.31 1.49 1.61 2.26 1.61 1.70 2.42 1.53 1.64 2.38 1.74 1.56 2.24 1.65 1.72 2.45 1.48 1.66 2.34 1.59 1.66 2.41 1.57 1.64 2.29 2.32 1.56 1.65 1.29 1.81 2.54 1.59 1.67 2.39 1.59 1.65 2.38 1.61 1.70 2.23 1.66 1.75 2.52 1.53 1.67 2.31 1.57 1.68 2.42

STANDARD DEVIATION Low Si Med Si High Si 0.013 0.021 0.026 0.013 0.000 0.007 0.008 0.019 0.019 0.033 0.046 0.061 0.013 0.015 0.008 0.010 0.013 0.012 0.019 0.029 0.047 0.034 0.029 0.005 0.007 0.007 0.018 0.011 0.027 0.117 0.080 0.096 0.023 0.038 0.018 0.009 0.008 0.015 0.017 0.020 0.021 0.021 0.021 0.029 0.011 0.011 0.004 0.011 0.020 0.024 0.008 0.015 0.015 0.008 0.004 0.009 0.011 0.010 0.029 0.019 0.008 0.017 0.015 0.024 0.023 0.067 0.066 0.039 0.012 0.008 0.011 0.000 0.000 0.000 0.021 0.026 0.043 0.018 0.035 0.058 0.017 0.024 0.025 0.019 0.005 0.029 0.011 0.011 0.021 0.014 0.008 0.013 0.025 0.025 0.018 0.013 0.013 0.013

1.66 1.57 0.105 6.7

sr =Repeatability std dev 0.029 0.026 0.030

1.66 1.67 0.057 3.4

2.33 2.36 0.077 3.3

Page 6

CONSISTENCY CONSISTENCY BETWEEN LABS WITHIN LAB h = (lab avg - interlab avg) k = lab std dev / std dev of lab avgs / repeatability std dev Low Si Med Si High Si Low Si Med Si High Si -0.29 -0.18 0.78 0.45 0.81 0.87 0.38 0.70 0.26 0.45 0.00 0.23 0.00 0.00 -0.26 0.28 0.73 0.63 -0.10 -0.70 -0.52 1.14 1.77 2.03 k -1.05 -0.39 0.00 0.50 0.50 -0.29 -0.70 -0.78 0.28 0.38 0.43 -0.29 -0.18 0.39 0.41 0.73 0.97 -2.10 0.53 -2.34 1.62 1.31 0.97 0.19 0.00 0.26 0.17 0.27 0.23 2.19 1.23 0.91 0.62 0.42 0.90 -1.43 3.16 h -0.52 4.03 k 3.08 k 3.20 k 0.67 -0.70 -0.78 0.79 1.46 0.60 1.43 -0.35 -0.65 0.31 0.31 0.50 1.71 -0.18 -0.52 0.59 0.77 0.70 -0.29 0.35 0.65 0.72 0.81 0.97 0.19 0.35 0.26 0.38 0.42 0.13 -0.86 -1.23 -0.65 0.38 0.77 0.80 -0.76 -1.05 -1.30 0.28 0.58 0.50 0.38 0.53 0.78 0.28 0.15 0.30 -0.38 -0.53 0.26 0.38 0.38 0.97 1.62 -1.93 -1.56 0.66 0.31 0.57 0.76 0.88 1.17 0.52 0.92 0.77 -0.86 -0.18 -0.26 2.31 k 2.54 k 1.30 0.19 -0.18 0.65 0.41 0.31 0.37 0.00 -0.53 -0.910.00 0.00 0.00 0.00 -0.10 -0.35 -0.52 0.72 1.00 1.43 -2.67 h 2.46 2.34 0.62 1.35 1.93 k 0.19 0.00 0.39 0.59 0.92 0.83 0.19 -0.35 0.26 0.66 0.19 0.97 0.38 0.53 -1.69 0.38 0.42 0.70 0.86 1.40 2.08 0.48 0.31 0.43 -0.38 0.00 -0.65 0.86 0.96 0.60 0.00 0.18 0.78 0.45 0.50 0.43 0.00 0.00 0.00 0.00

|h| >2.64 indicates statistically significant variation between

33 labs.

k > 1.89 indicates statistically significant variation within lab for 33 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. Si 1.9 1.8

% Si

1.7 1.6 1.5 1.4 1.3

1

3

5

7

9

11

13

15

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab Number

Avg = 1.57%

Medium Conc. Si 2 1.9

% Si

1.8 1.7 1.6 1.5 1.4

1

3

5

7

9

11

13

15

17

19

Lab Number

Avg = 1.67%

High Conc. Si 2.8 2.7 2.6 % Si

2.5 2.4 2.3 2.2 2.1 2

1

3

Avg = 2.36%

5

7

9

11

13

15

17

19

21

23

25

27

29

31

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.

33


TABLE 2

ICRI REPORT NO 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

MANGANESE

AVERAGE STANDARD DEVIATION Low Mn Med MnHigh Mn Low Mn Med Mn High Mn 0.28 0.60 0.88 0.005 0.000 0.004 0.29 0.64 0.92 0.005 0.004 0.011 0.28 0.60 0.89 0.000 0.007 0.011 0.30 0.65 0.93 0.004 0.009 0.012 0.29 0.63 0.002 0.005 0.28 0.60 0.84 0.000 0.009 0.009 0.28 0.62 0.89 0.005 0.005 0.004 0.27 0.60 0.82 0.004 0.009 0.015 0.29 0.62 0.91 0.000 0.000 0.000 0.28 0.61 0.87 0.005 0.007 0.005 0.29 0.68 0.80 0.024 0.019 0.050 0.27 0.60 0.90 0.002 0.004 0.008 0.27 0.60 0.85 0.000 0.004 0.008 0.27 0.60 0.86 0.000 0.004 0.005 0.26 0.61 0.87 0.004 0.011 0.005 0.29 0.60 0.85 0.005 0.007 0.007 0.30 0.66 0.94 0.000 0.004 0.010 0.28 0.57 0.83 0.004 0.007 0.008 0.29 0.60 0.87 0.000 0.000 0.004 0.28 0.59 0.85 0.005 0.005 0.005 0.28 0.60 0.94 0.000 0.000 0.005 0.28 0.61 0.91 0.005 0.005 0.010 0.28 0.59 0.87 0.009 0.014 0.022 0.26 0.57 0.90 0.004 0.005 0.005 0.28 0.61 0.88 0.000 0.000 0.000 0.28 0.60 0.86 0.004 0.004 0.007 0.27 0.58 0.81 0.004 0.004 0.005 0.30 0.65 0.97 0.024 0.049 0.076 0.28 0.65 0.83 0.004 0.009 0.020 0.07 0.59 0.89 0.005 0.021 0.023 0.27 0.60 0.87 0.000 0.000 0.007 0.24 0.63 0.86 0.013 0.026 0.024 0.28 0.62 0.93 0.000 0.004 0.004

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

Target Interlab Avg Std Dev of Avg Coef of variation

0.29 0.27 0.038 14.1

0.60 0.61 0.025 4.1

0.92 0.88 0.040 4.5

sr =Repeatability std dev 0.007 0.012 0.019

Page 8

CONSISTENCY CONSISTENCY BETWEEN LABS WITHIN LAB h = (lab avg - interlab avg) k = lab std dev / std dev of lab avgs / repeatability std dev Low Mn Med Mn High Mn Low Mn Med Mn High Mn 0.26 -0.40 0.00 0.71 0.00 0.21 0.53 1.20 1.00 0.71 0.33 0.58 0.26 -0.40 0.25 0.00 0.58 0.58 0.79 1.60 1.25 0.57 0.75 0.63 0.53 0.80 # 0.29 0.42 0.26 -0.40 -1.00 0.00 0.75 0.47 0.26 0.40 0.25 0.71 0.42 0.21 0.00 -0.40 -1.50 0.57 0.75 0.79 0.53 0.40 0.75 0.00 0.00 0.00 0.26 0.00 -0.25 0.71 0.58 0.26 0.53 2.80 h -2.00 3.43 k 1.58 2.63 0.00 -0.40 0.50 0.29 0.33 0.42 0.00 -0.40 -0.75 0.00 0.33 0.42 0.00 -0.40 -0.50 0.00 0.33 0.26 -0.26 0.00 -0.25 0.57 0.92 0.26 0.53 -0.40 -0.75 0.71 0.58 0.37 0.79 2.00 1.50 0.00 0.33 0.53 0.26 -1.60 -1.25 0.57 0.58 0.42 0.53 -0.40 -0.25 0.00 0.00 0.21 0.26 -0.80 -0.75 0.71 0.42 0.26 0.26 -0.40 1.50 0.00 0.00 0.26 0.26 0.00 0.75 0.71 0.42 0.53 0.26 -0.80 -0.25 1.29 1.17 1.16 -0.26 -1.60 0.50 0.57 0.42 0.26 0.26 0.00 0.00 0.00 0.00 0.00 0.26 -0.40 -0.50 0.57 0.33 0.37 0.00 -1.20 -1.75 0.57 0.33 0.26 0.79 1.60 2.25 3.43 k 4.08 k 4.00 0.26 1.60 -1.25 0.57 0.75 1.05 -5.26 h -0.80 0.25 0.71 1.75 1.21 0.00 -0.40 -0.25 0.00 0.00 0.37 -0.79 0.80 -0.50 1.86 2.17 k 1.26 0.26 0.40 1.25 0.00 0.33 0.21 # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # #

|h| >2.64 indicates statistically significant variation between

33 labs.

#

k

k

# # # # # # # # # # # # # #

k > 1.89 indicates statistically significant variation within lab for 33 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO. 641 4/9/13

Low Conc. Mn 0.35 0.3

% Mn

0.25 0.2 0.15 0.1

1

3

5

7

9

11

13

15

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Avg = 0.27% Lab Number

Medium Conc. Mn 0.75 0.70

% Mn

0.65 0.60 0.55 0.50 0.45 0.40

1

3

5

7

9

11

13

15

17

19

Lab Number

Avg = 0.61%

High Conc. Mn 1.1 1

% Mn

0.9 0.8 0.7 0.6 0.5

1

3

Avg = 0.88%

5

7

9

11

13

15

17

19

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.


TABLE 3

ICRI REPORT NO 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

SULFUR

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

Target Interlab Avg Std Dev of Avg Coef of variation

AVERAGE Low S Med S High S 0.010 0.009 0.047 0.025 0.011 0.045 0.004 0.008 0.031 0.013 0.008 0.036 0.008 0.012 0.037 0.010 0.010 0.043 0.016 0.013 0.039

STANDARD DEVIATION Low S Med S High S 0.002 0.001 0.001 0.002 0.001 0.001 0.001 0.001 0.000 0.002 0.001 0.001 0.002 0.003 0.003 0.001 0.001 0.001 0.003 0.002 0.002

0.009 0.011 0.020 0.015 0.016 0.016 0.012 0.019 0.015 0.008 0.011 0.006 0.015 0.014

0.002 0.008 0.009 0.008 0.009 0.009 0.008 0.013 0.010 0.006 0.007 0.001 0.010 0.017

0.040 0.030 0.048 0.037 0.042 0.039 0.039 0.050 0.048 0.031 0.040 0.035 0.043 0.026

0.001 0.002 0.001 0.002 0.004 0.002 0.000 0.002 0.002 0.001 0.001 0.001 0.005 0.002

0.001 0.001 0.001 0.002 0.001 0.001 0.001 0.002 0.001 0.001 0.001 0.000 0.002 0.001

0.001 0.002 0.004 0.001 0.002 0.001 0.001 0.001 0.002 0.000 0.002 0.001 0.002 0.001

0.011 0.014 0.008 0.011 0.014 0.077 0.014 0.010 0.010

0.006 0.004 0.006 0.007 0.007 0.025 0.011 0.008 0.012

0.040 0.043 0.032 0.044 0.043 0.103 0.042 0.040 0.035

0.000 0.002 0.002 0.002 0.002 0.019 0.003 0.002 0.001

0.000 0.003 0.001 0.006 0.001 0.004 0.001 0.001 0.001

0.000 0.002 0.002 0.003 0.001 0.003 0.001 0.001 0.005

0.010 0.015 0.013 86.7

0.011 0.009 0.004 44.4

0.044 0.042 0.013 31.0

sr =Repeatability std dev 0.004 0.002 0.002

Page 10

CONSISTENCY BETWEEN LABS h = (lab avg - interlab avg) / std dev of lab avgs Low S Med S High S -0.38 0.00 0.38 0.77 0.50 0.23 -0.85 -0.25 -0.85 -0.15 -0.25 -0.46 -0.54 0.75 -0.38 -0.38 0.25 0.08 0.08 1.00 -0.23 # # -0.46 -1.75 -0.15 -0.31 -0.25 -0.92 0.38 0.00 0.46 0.00 -0.25 -0.38 0.08 0.00 0.00 0.08 0.00 -0.23 -0.23 -0.25 -0.23 0.31 1.00 0.62 0.00 0.25 0.46 -0.54 -0.75 -0.85 -0.31 -0.50 -0.15 -0.69 -2.00 -0.54 0.00 0.25 0.08 -0.08 2.00 -1.23 # # # # -0.31 -0.75 -0.15 -0.08 -1.25 0.08 -0.54 -0.75 -0.77 -0.31 -0.50 0.15 -0.08 -0.50 0.08 4.77 h 4.00 h 4.69 -0.08 0.50 0.00 -0.38 -0.25 -0.15 -0.38 0.75 -0.54 # # # # # # # # # # # # # # # # # # # # # # # # # # # #

|h| >2.64 indicates statistically significant variation between

30 labs.

#

# #

h

# # # # # # # # # # # # # #

CONSISTENCY WITHIN LAB k = lab std dev / repeatability std dev Low S Med S High S 0.50 0.50 0.50 0.50 0.50 0.50 0.25 0.50 0.00 0.50 0.50 0.50 0.50 1.50 1.50 0.25 0.50 0.50 0.75 1.00 1.00 # # # 0.25 0.50 0.50 0.50 0.50 1.00 0.25 0.50 2.00 k 0.50 1.00 0.50 1.00 0.50 1.00 0.50 0.50 0.50 0.00 0.50 0.50 0.50 1.00 0.50 0.50 0.50 1.00 0.25 0.50 0.00 0.25 0.50 1.00 0.25 0.00 0.50 1.25 1.00 1.00 0.50 0.50 0.50 # # # # # # 0.00 0.00 0.00 0.50 1.50 1.00 0.50 0.50 1.00 0.50 3.00 k 1.50 0.50 0.50 0.50 4.75 k 2.00 k 1.50 0.75 0.50 0.50 0.50 0.50 0.50 0.25 0.50 2.50 k # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # #

k > 1.89 indicates statistically significant variation within lab for 30 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. S 0.12 0.1

%S

0 08 0.08 0.06 0.04 0.02 0

1

3

5

7

9

11

13

Avg = 0.015%

15

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab Number

Medium Conc. S 0.035 0.03 0.025

%S

0.02 0.015 0.01 0.005 0

1

3

5

7

9

11

13

Avg = 0.009%

15

17

19

Lab Number

High Conc. S 0.11 0.1 0.09 0.08 %S

0 07 0.07 0.06 0.05 0.04 0.03 0.02

1

3

Avg = 0.042%

5

7

9

11

13

15

17

19

21

23

25

27

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.

29

31

33


TABLE 4

ICRI REPORT NO 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

PHOSPHORUS

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

Target Interlab Avg Std Dev of Avg Coef of variation

AVERAGE Low P Med P High P 0.02 0.08 0.08 0.03 0.09 0.10 0.03 0.09 0.10 0.03 0.10 0.11 0.03 0.09 0.03 0.08 0.11 0.03 0.09 0.10 0.03 0.11 0.10 0.03 0.08 0.10 0.03 0.08 0.10 0.03 0.08 0.10 0.03 0.08 0.10 0.04 0.08 0.11 0.04 0.08 0.10 0.03 0.09 0.10 0.04 0.10 0.11 0.03 0.09 0.10 0.03 0.10 0.10 0.03 0.08 0.09 0.03 0.09 0.10 0.03 0.09 0.10 0.03 0.07 0.10 0.06 0.11 0.10 0.03 0.10 0.10 0.03 0.08 0.10 0.02 0.07 0.09 0.03 0.06 0.08 0.02 0.07 0.09 0.03 0.09 0.11 0.04 0.08 0.11 0.03 0.08 0.10 0.03 0.08 0.10 0.02 0.09 0.10

STANDARD DEVIATION Low P Med P High P 0.000 0.005 0.005 0.000 0.000 0.000 0.000 0.001 0.001 0.000 0.005 0.005 0.000 0.004 0.000 0.002 0.003 0.000 0.005 0.002 0.000 0.005 0.004 0.000 0.000 0.005 0.000 0.005 0.004 0.000 0.000 0.000 0.000 0.000 0.005 0.000 0.004 0.004 0.000 0.004 0.000 0.005 0.005 0.000 0.004 0.005 0.008 0.000 0.000 0.005 0.000 0.000 0.005 0.000 0.004 0.005 0.007 0.011 0.011 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.005 0.005 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.005 0.005 0.005 0.005 0.000 0.005 0.000 0.005 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.009

0.03 0.03 0.007 23.3

sr =Repeatability std dev 0.002 0.004 0.004

0.09 0.09 0.011 12.2

0.11 0.10 0.007 7.0

Page 12

CONSISTENCY CONSISTENCY BETWEEN LABS WITHIN LAB h = (lab avg - interlab avg) k = lab std dev / std dev of lab avgs / repeatability std dev Low P Med P High P Low P Med P High P -1.43 -0.91 -2.86 h 0.00 1.25 1.25 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.25 0.25 0.00 0.91 1.43 0.00 1.25 1.25 0.00 ## -1.43 0.00 # 1.00 0.00 -0.91 1.43 0.00 0.50 0.75 0.00 0.00 0.00 0.00 1.25 0.50 0.00 1.82 0.00 0.00 1.25 1.00 0.00 -0.91 0.00 0.00 0.00 1.25 0.00 -0.91 0.00 0.00 1.25 1.00 0.00 -0.91 0.00 0.00 0.00 0.00 0.00 -0.91 0.00 0.00 0.00 1.25 1.43 -0.91 1.43 0.00 1.00 1.00 1.43 -0.91 0.00 0.00 1.00 0.00 0.00 0.00 0.00 2.50 k 1.25 0.00 1.43 0.91 1.43 2.00 k 1.25 2.00 k 0.00 0.00 0.00 0.00 0.00 1.25 0.00 0.91 0.00 0.00 0.00 1.25 0.00 -0.91 -1.43 0.00 1.00 1.25 0.00 0.00 0.00 3.50 k 2.75 k 2.75 k 0.00 0.00 0.00 0.00 1.00 0.00 0.00 -1.82 0.00 0.00 0.00 0.00 4.29 h 1.82 0.00 0.00 1.25 1.25 0.00 0.91 0.00 0.00 0.00 1.00 0.00 -0.91 0.00 0.00 0.00 0.00 -1.43 -1.82 -1.43 0.00 0.00 0.00 0.00 -2.73 h -2.86 h 0.00 0.00 1.25 -1.43 -1.82 -1.43 2.50 k 1.25 1.25 0.00 0.00 1.43 2.50 k 0.00 1.25 1.43 -0.91 1.43 0.00 1.25 1.25 0.00 -0.91 0.00 0.00 0.00 0.00 0.00 -0.91 0.00 0.00 0.00 0.00 -1.43 0.00 0.00 0.00 2.00 k 2.25 k # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # #

|h| >2.64 indicates statistically significant variation between

33 labs.

k > 1.89 indicates statistically significant variation within lab for 33 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. P 0.070 0.060 0.050

%P

0.040 0.030 0.020 0.010

1

3

5

7

9

11

13

15

Avg = 0.03%

17

19

21

23

25

27

29

31

33

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab No Medium Conc. P

0.13 0.11 0.09

%P

0.07 0.05 0.03 0.01

1

3

5

7

9

11

13

15

17

Lab Number

Avg = 0.09%

High Conc. P 0.13 0.12 0.11

%P

0.1 0.09 0.08 0.07 0.06 0.05

1

3

Avg = 0.10%

5

7

9

11

13

15

17

19

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.


TABLE 5

ICRI REPORT NO 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

CHROMIUM

AVERAGE Low Cr Med Cr High Cr 0.10 0.22 0.26 0.09 0.22 0.27 0.09 0.22 0.27 0.11 0.22 0.28 0.10 0.22 0.10 0.23 0.28 0.09 0.23 0.29 0.10 0.22 0.26 0.09 0.22 0.28 0.09 0.21 0.26 0.09 0.23 0.25 0.10 0.22 0.24 0.10 0.22 0.27 0.10 0.23 0.28 0.08 0.19 0.25 0.10 0.24 0.29 0.09 0.22 0.27 0.09 0.23 0.30 0.09 0.21 0.27 0.10 0.23 0.32 0.10 0.22 0.29 0.10 0.23 0.29 0.09 0.22 0.29 0.10 0.22 0.29 0.10 0.23 0.28 0.10 0.23 0.28 0.08 0.21 0.27 0.09 0.23 0.29 0.08 0.21 0.29 0.08 0.21 0.27 0.11 0.25 0.31 0.10 0.22 0.26 0.08 0.21 0.27

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

Target Interlab Avg Std Dev of Avg Coef of variation

0.10 0.09 0.008 8.9

0.23 0.22 0.011 5.0

0.30 0.28 0.017 6.1

h = (lab avg - interlab avg) k = lab std dev STANDARD DEVIATION / std dev of lab avgs / repeatability std dev Low Cr Med Cr High Cr Low Cr Med Cr High Cr Low Cr Med Cr High Cr 0.004 0.000 0.004 1.25 0.00 -1.18 1.00 0.00 0.50 0.000 0.004 0.000 0.00 0.00 -0.59 0.00 0.80 0.00 0.002 0.005 0.000 0.00 0.00 -0.59 0.50 1.00 0.00 0.004 0.004 0.004 2.50 0.00 0.00 1.00 0.80 0.50 0.000 0.000 1.25 0.00 # 0.00 0.00 # 0.003 0.002 0.000 1.25 0.91 0.00 0.75 0.40 0.00 0.000 0.003 0.005 0.00 0.91 0.59 0.00 0.60 0.63 0.000 0.009 0.011 1.25 0.00 -1.18 0.00 1.80 1.38 0.000 0.000 0.005 0.00 0.00 0.00 0.00 0.00 0.63 0.000 0.004 0.004 0.00 -0.91 -1.18 0.00 0.80 0.50 0.005 0.012 0.025 0.00 0.91 -1.76 1.25 2.40 k 3.13 k 0.002 0.004 0.025 1.25 0.00 -2.35 0.50 0.80 3.13 k 0.000 0.000 0.000 1.25 0.00 -0.59 0.00 0.00 0.00 0.000 0.004 0.005 1.25 0.91 0.00 0.00 0.80 0.63 0.009 0.005 0.000 -1.25 -2.73 h -1.76 2.25 k 1.00 0.00 0.000 0.004 0.004 1.25 1.82 0.59 0.00 0.80 0.50 0.000 0.005 0.005 0.00 0.00 -0.59 0.00 1.00 0.63 0.000 0.004 0.004 0.00 0.91 1.18 0.00 0.80 0.50 0.004 0.000 0.004 0.00 -0.91 -0.59 1.00 0.00 0.50 0.000 0.005 0.005 1.25 0.91 2.35 0.00 1.00 0.63 0.000 0.000 0.000 1.25 0.00 0.59 0.00 0.00 0.00 0.000 0.004 0.005 1.25 0.91 0.59 0.00 0.80 0.63 0.009 0.005 0.012 0.00 0.00 0.59 2.25 k 1.00 1.50 0.004 0.004 0.007 1.25 0.00 0.59 1.00 0.80 0.88 0.000 0.000 0.000 1.25 0.91 0.00 0.00 0.00 0.00 0.004 0.007 0.011 1.25 0.91 0.00 1.00 1.40 1.38 0.000 0.004 0.004 -1.25 -0.91 -0.59 0.00 0.80 0.50 0.000 0.005 0.006 0.00 0.91 0.59 0.00 1.00 0.75 0.013 0.009 0.011 -1.25 -0.91 0.59 3.25 k 1.80 1.38 0.005 0.005 0.000 -1.25 -0.91 -0.59 1.25 1.00 0.00 0.000 0.007 0.005 2.50 2.73 h 1.76 0.00 1.40 0.63 0.005 0.008 0.008 1.25 0.00 -1.18 1.25 1.60 1.00 0.000 0.000 0.004 -1.25 -0.91 -0.59 0.00 0.00 0.50 # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # #

sr =Repeatability std dev 0.004 0.005 0.008

Page 14

|h| >2.64 indicates statistically significant variation between

33 labs.

k > 1.89 indicates statistically significant variation within lab for 33 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. Cr 0.120 0.110 0.100 % Cr

0.090 0.080 0.070 0.060

1

3

5

7

9

11

13

Avg = 0.09%

15

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab Number

Medium Conc. Cr 0.28 0.26 0.24 0.22 % Cr

0.2 0.18 0.16 0.14 0.12 0.1

1

3

5

7

9

11

13

Avg = 0.22%

15

17

19

Lab Number

High Conc. Cr 0.33 0.31 0.29 0.27 % Cr

0.25 0.23 0.21 0.19 0.17 0.15

1

3

Avg = 0.28%

5

7

9

11

13

15

17

19

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.


TABLE 6

ICRI REPORT NO 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

COPPER

CONSISTENCY CONSISTENCY BETWEEN LABS WITHIN LAB h = (lab avg - interlab avg) k = lab std dev AVERAGE STANDARD DEVIATION / std dev of lab avgs / repeatability std dev Low CuMed CuHigh Cu Low Cu Med Cu High Cu Low Cu Med Cu High Cu Low Cu Med Cu High Cu 0.03 0.11 1.08 0.004 0.005 0.033 -1.67 1.11 1.30 1.33 1.67 1.50 0.03 0.11 0.91 0.000 0.000 0.005 -1.67 1.11 -0.54 0.00 0.00 0.23 0.04 0.10 0.97 0.000 0.003 0.004 0.00 0.00 0.11 0.00 1.00 0.18 0.03 0.10 0.87 0.005 0.004 0.012 -1.67 0.00 -0.98 1.67 1.33 0.55 0.03 0.10 0.005 0.000 -1.67 0.00 # 1.67 0.00 # 0.04 0.11 0.94 0.000 0.000 0.011 0.00 1.11 -0.22 0.00 0.00 0.50 0.03 0.10 0.96 0.000 0.004 0.016 -1.67 0.00 0.00 0.00 1.33 0.73 0.03 0.10 0.94 0.000 0.000 0.017 -1.67 0.00 -0.22 0.00 0.00 0.77 0.04 0.11 0.96 0.000 0.000 0.005 0.00 1.11 0.00 0.00 0.00 0.23 0.03 0.11 0.95 0.005 0.005 0.016 -1.67 1.11 -0.11 1.67 1.67 0.73 0.05 0.11 0.87 0.007 0.005 0.057 1.67 1.11 -0.98 2.33 k 1.67 2.59 k 0.04 0.11 0.94 0.000 0.000 0.004 0.00 1.11 -0.22 0.00 0.00 0.18 0.04 0.09 0.92 0.004 0.000 0.011 0.00 -1.11 -0.43 1.33 0.00 0.50 0.04 0.09 0.91 0.000 0.000 0.043 0.00 -1.11 -0.54 0.00 0.00 1.95 k 0.04 0.10 1.02 0.000 0.008 0.004 0.00 0.00 0.65 0.00 2.67 k 0.18 0.04 0.11 0.91 0.000 0.000 0.022 0.00 1.11 -0.54 0.00 0.00 1.00 0.04 0.12 1.01 0.000 0.004 0.045 0.00 2.22 0.54 0.00 1.33 2.05 k 0.04 0.11 1.07 0.000 0.000 0.015 0.00 1.11 1.20 0.00 0.00 0.68 0.04 0.11 1.01 0.000 0.001 0.011 0.00 1.11 0.54 0.00 0.33 0.50 0.04 0.11 0.87 0.000 0.000 0.015 0.00 1.11 -0.98 0.00 0.00 0.68 0.03 0.09 0.62 0.005 0.009 0.011 -1.67 -1.11 -3.70 h 1.67 3.00 k 0.50 0.04 0.11 1.14 0.005 0.004 0.040 0.00 1.11 1.96 1.67 1.33 1.82 0.03 0.11 1.02 0.005 0.004 0.034 -1.67 1.11 0.65 1.67 1.33 1.55 0.02 0.09 1.08 0.000 0.000 0.014 -3.33 h -1.11 1.30 0.00 0.00 0.64 0.04 0.11 0.95 0.000 0.000 0.000 0.00 1.11 -0.11 0.00 0.00 0.00 0.03 0.09 0.96 0.000 0.000 0.005 -1.67 -1.11 0.00 0.00 0.00 0.23 0.04 0.10 1.05 0.008 0.004 0.016 0.00 0.00 0.98 2.67 k 1.33 0.73 0.03 0.10 0.95 0.000 0.000 0.013 -1.67 0.00 -0.11 0.00 0.00 0.59 0.04 0.12 0.97 0.000 0.000 0.008 0.00 2.22 0.11 0.00 0.00 0.36 0.04 0.11 1.08 0.005 0.005 0.034 0.00 1.11 1.30 1.67 1.67 1.55 0.04 0.11 0.99 0.000 0.000 0.000 0.00 1.11 0.33 0.00 0.00 0.00 0.03 0.11 0.96 0.000 0.005 0.018 -1.67 1.11 0.00 0.00 1.67 0.82 0.03 0.09 0.93 0.004 0.000 0.016 -1.67 -1.11 -0.33 1.33 0.00 0.73 # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## # # # # # ## #

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

Target Interlab Avg Std Dev of Avg Coef of variation

0.04 0.04 0.006 15.0

0.11 0.10 0.009 9.0

0.99 0.96 0.092 9.6

sr =Repeatability std dev 0.003 0.003 0.022

Page 16

|h| >2.64 indicates statistically significant variation between

33 labs.

k > 1.89 indicates statistically significant variation within lab for 33 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. Cu 0.065 0.06 0.055 0.05 % Cu

0.045 0.04 0.035 0.03 0.025 0.02

1

3

5

7

9

11

13

15

17

19

21

23

25

27

29

31

33

Lab Number

Avg = 0.04%

Medium Conc. Cu 0.14 0.12

% Cu

0.1 0.08 0.06 0.04 0 02 0.02

1

3

5

7

9

11

13

15

Avg = 0.10%

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab Number

High Conc. Cu 1.4 1.2

% Cu

1 0.8 0.6 0.4 0.2

1

3

Avg = 0.96%

5

7

9

11

13

15

17

19

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.


TABLE 7

ICRI REPORT NO 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

TIN

AVERAGE Low Sn Med Sn High Sn 0.001 0.014 0.047 0.003 0.017 0.053 0.015 0.053 0.015 0.034 0.014 0.002 0.018 0.052 0.014 0.029 0.063

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

0.003 0.001 0.005

0.004 0.004 0.002 0.002

0.020 0.010 0.020 0.013 0.015 0.015 0.013 0.013 0.018 0.016 0.018 0.014 0.017 0.014 0.010 0.014 0.015 0.018

0.059 0.033 0.039 0.043 0.051 0.051 0.049 0.030 0.050 0.056 0.063 0.048 0.052 0.033 0.036 0.038 0.058 0.055

0.001 0.058

0.014 0.030

0.005

0.018 0.016

0.052 0.171 0.171 0.049 0.005 0.061

0.021 0.016 0.0045 28.1

0.050 0.055 0.0337 61.3

0.003 0.006 0.002 0.001 0.000 0.001 0.002

Target Interlab Avg Std Dev of Avg Coef of variation

0.002 0.006 0.0122 203.3

STANDARD DEVIATION Low Sn Med Sn High Sn 0.0000 0.0013 0.0008 0.0000 0.0008 0.0007 0.0009 0.0022 0.0116 0.0172 0.0004 0.0000 0.0007 0.0011 0.0009 0.0019 0.0014 0.0000 0.0000 0.0013

0.0018 0.0000 0.0000 0.0000

0.0000 0.0000 0.0060 0.0000 0.0005 0.0005 0.0008 0.0009 0.0013 0.0004 0.0004 0.0005 0.0000 0.0055 0.0009 0.0000 0.0000 0.0000

0.0000 0.0005 0.0043 0.0000 0.0008 0.0008 0.0014 0.0040 0.0060 0.0004 0.0013 0.0019 0.0018 0.0031 0.0021 0.0005 0.0004 0.0004

0.0009 0.0099

0.0025 0.0174

0.0000

0.0005

0.0010 0.0128 0.0528 0.0007 0.0035 0.0011

0.0005 0.0000 0.0004 0.0000 0.0004 0.0000

0.0008

sr =Repeatability std dev 0.0034 0.0037 0.0106

Page 18

CONSISTENCY CONSISTENCY BETWEEN LABS WITHIN LAB h = (lab avg - interlab avg) k = lab std dev / std dev of lab avgs / repeatability std dev Low Sn Med Sn High Sn Low Sn Med Sn High Sn -0.41 -0.44 -0.24 0.00 0.35 0.08 -0.25 0.22 -0.06 0.00 0.22 0.07 -0.22 -0.06 0.24 0.21 0.00 0.00 -0.62 3.41 k 1.62 -0.44 0.11 0.00 -0.33 0.44 -0.09 0.00 0.19 0.10 0.00 2.89 h 0.24 0.26 0.51 0.13 0.00 0.00 0.00 0.89 0.12 0.00 0.00 0.00 -0.41 -1.33 -0.65 0.00 0.00 0.05 -0.08 0.89 -0.47 0.38 1.62 0.41 -0.67 -0.36 0.00 0.00 -0.22 -0.12 0.14 0.08 0.00 -0.22 -0.12 0.14 0.08 -0.25 -0.67 -0.18 0.15 0.22 0.13 0.00 -0.67 -0.74 0.00 0.24 0.38 -0.33 0.44 -0.15 0.12 0.35 0.57 -0.41 0.00 0.03 0.00 0.11 0.04 -0.49 0.44 0.24 0.00 0.11 0.12 -0.41 -0.44 -0.21 0.12 0.14 0.18 -0.33 0.22 -0.09 0.00 0.00 0.17 -0.44 -0.65 1.49 0.29 -0.16 -1.33 -0.56 0.53 0.24 0.20 -0.16 -0.44 -0.50 0.00 0.00 0.05 -0.33 -0.22 0.09 0.00 0.00 0.04 -0.33 0.44 0.00 0.00 0.00 0.04 0.00 0.00 0.00 0.00 -0.41 -0.44 -0.09 0.26 0.68 0.09 4.26 h 3.11 h 3.44 h 2.91 k 4.70 k 1.21 0.00 0.00 3.44 h 4.98 k -0.08 0.44 -0.18 0.00 0.14 0.07 0.00 0.00 -1.48 0.33 0.18 0.22 0.10

|h| >2.64 indicates statistically significant variation between

30 labs.

k > 1.89 indicates statistically significant variation within lab for 30 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. Sn 0.08 0.07 0.06

% Sn

0.05 0.04 0.03 0.02 0.01 0

1

3

5

7

9

11

13

Avg  = 0.006%

15

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab Number

Medium Conc. Sn 0.051 0.046 0.041 0.036 % Sn

0.031 0.026 0.021 0.016 0.011 0.006 0.001

1

3

5

7

9

11

13

Avg = 0.016%

15

17

19

Lab Number

High Conc. Sn 0.26 0.21

% Sn

0.16 0.11 0.06 0.01

1

3

Avg = 0.055%

5

7

9

11

13

15

17

19

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.


TABLE 8

ICRI REPORT NO 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

MAGNESIUM

AVERAGE Low Mg Med Mg High Mg 0.001 0.037 0.042 0.050 0.041 0.030 0.037 0.044 0.045 0.027 0.000 0.038 0.049 0.001 0.045 0.047 0.005 0.042 0.035 0.002 0.033 0.036 0.038 0.053 0.005 0.040 0.038 0.000 0.052 0.053 0.055 0.060 0.060 0.073 0.001 0.044 0.037 0.007 0.047 0.043 0.001 0.040 0.044 0.002 0.035 0.035 0.041 0.043 0.001 0.038 0.044

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

0.001 0.002

0.004 0.000

Target Interlab Avg Std Dev of Avg Coef of variation

0.008 0.002 0.0021 105.0

STANDARD DEVIATION Low Mg Med Mg High Mg 0.0001 0.0015 0.0019 0.0025 0.0009 0.0023 0.0005 0.0016 0.0021 0.0028 0.0000 0.0014 0.0031 0.0000 0.0050 0.0018 0.0009 0.0011 0.0026 0.0009 0.0013 0.0017 0.0019 0.0043 0.0046 0.0039 0.0000 0.0043 0.0022 0.0053 0.0025 0.0027 0.0025 0.0005 0.0015 0.0009 0.0005 0.0038 0.0040 0.0000 0.0027 0.0033 0.0000 0.0011 0.0019 0.0018 0.0029 0.0000 0.0029 0.0041

CONSISTENCY CONSISTENCY BETWEEN LABS WITHIN LAB h = (lab avg - interlab avg) k = lab std dev / std dev of lab avgs / repeatability std dev Low Mg Med Mg High Mg Low Mg Med Mg High Mg -0.48 -0.50 -0.22 0.14 0.44 0.54 # 0.79 -0.33 # 0.74 0.26 # -1.19 -0.76 # 0.68 0.14 # 0.20 0.11 # 0.47 0.60 # -1.49 # # 0.82 ## -0.95 -0.40 0.54 0.00 0.41 0.89 -0.48 0.30 0.33 0.00 1.47 0.51 1.43 0.00 -0.98 1.29 0.32 0.74 0.00 -0.89 -0.87 1.29 0.38 0.49 # -0.40 0.98 0.56 1.23 1.43 -0.20 -0.65 0.00 1.35 1.11 -0.95 0.99 0.98 0.00 1.26 0.63 # 1.29 1.74 # 1.56 0.71 # 1.78 3.15 h # 0.79 0.71 -0.48 0.20 -0.76 0.71 0.44 0.26 2.38 0.50 -0.11 0.71 1.12 1.14 -0.48 -0.20 0.00 0.00 0.79 0.94 0.00 -0.69 -0.98 0.00 0.32 0.54 # -0.10 -0.11 # 0.53 0.83 -0.48 -0.40 0.00 0.00 0.85 1.17 # ## # # # ## # -0.40 -0.65 # 1.00 0.80 # -0.59 -0.98 # 1.32 0.83 -0.48 0.40 0.65 0.00 1.56 1.17 0.00 -0.99 -1.96 0.00 0.00 0.11 # ## # # # ## # -0.59 -0.33 # 0.56 0.60 0.95 -0.79 -1.09 3.00 k 1.74 0.89 -0.95 0.00 -0.54 0.00 0.41 0.43 # 3.76 h 0.98 # 2.62 k 2.63 k # -0.89 -0.76 0.41 1.06 # -0.40 0.33 # 0.32 0.54 # -0.20 0.76 # 1.09 2.63 k # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ## # ## # # # ##

0.038 0.036 0.046 0.032

0.038 0.035 0.050 0.026

0.0034 0.0045 0.0000 0.0053 0.0000 0.0000

0.0028 0.0029 0.0041 0.0004

0.036 0.034 0.042 0.080 0.033 0.038 0.040

0.041 0.034 0.039 0.053 0.037 0.047 0.051

0.0019 0.0021 0.0059 0.0000 0.0014 0.0089 0.0014 0.0011 0.0037

0.0021 0.0031 0.0015 0.0092 0.0037 0.0019 0.0092

0.041 0.042 0.0101 24.0

0.055 0.044 0.0092 20.9

sr =Repeatability std dev significant variation between 0.0007 0.0034 0.0035 33 labs.

|h| >2.64 indicates statistically

Page 20

k > 1.89 indicates statistically significant variation within lab for 33 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. Mg 0.008

0.006

% Mg

0.004

0.002

0.000

1

3

5

7

9

11

13

15

Avg = 0.002%

17

19

21

23

25

27

29

31

33

Lab Number

Medium Conc. Mg 0.1 0.09 0.08 0.07 % Mg

0.06 0.05 0.04 0 03 0.03 0.02 0.01

1

3

5

7

9

11

13

Avg = 0.042%

15

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab Number

High Conc. Mg 0.08 0.07

% Mg

0.06 0.05 0.04 0.03 0.02

1

3

Avg = 0.044%

5

7

9

11

13

15

17

19

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.


TABLE 9

ICRI REPORT NO. 641 4/9/13 INTERLAB SPECTROMETER PROFICIENCY TESTING

ALUMINUM

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

Target Interlab Avg Std Dev of Avg Coef of variation

AVERAGE Low Al Med Al High Al 0.011 0.011 0.030 0.004 0.005 0.042 0.003 0.004 0.036 0.005 0.004 0.035 0.005 0.005 0.004 0.041 0.005 0.005 0.038 0.004 0.003 0.035 0.003 0.003 0.041 0.006 0.005 0.039 0.004 0.003 0.033 0.004 0.003 0.036 0.004 0.004 0.038 0.004 0.003 0.038 0.007 0.007 0.039 0.008 0.008 0.035 0.005 0.004 0.034 0.033 0.006 0.005 0.038 0.005 0.004 0.038 0.006 0.005 0.041 0.003 0.002 0.035 0.001 0.001 0.038 0.013 0.013 0.031 0.005 0.004 0.039 0.004 0.003 0.043 0.007 0.007 0.030 0.002 0.001 0.054 0.004 0.005 0.032

STANDARD DEVIATION Low Al Med Al High Al 0.0000 0.0000 0.0004 0.0000 0.0005 0.0009 0.0005 0.0004 0.0011 0.0000 0.0000 0.0004 0.0004 0.0004 0.0004 0.0004 0.0008 0.0005 0.0018 0.0000 0.0005 0.0004 0.0005 0.0000 0.0005 0.0000 0.0005 0.0014 0.0006 0.0011 0.0027 0.0005 0.0004 0.0004 0.0000 0.0005 0.0005 0.0000 0.0000 0.0004 0.0005 0.0008 0.0011 0.0004 0.0009 0.0004 0.0004 0.0000 0.0004 0.0005 0.0004 0.0000 0.0008 0.0005 0.0004 0.0025 0.0016 0.0009 0.0008 0.0005 0.0007 0.0010 0.0000 0.0000 0.0024 0.0000 0.0004 0.0004 0.0000 0.0000 0.0000 0.0000 0.0000 0.0011 0.0004 0.0000 0.0004 0.0021 0.0012 0.0010 0.0005 0.0005 0.0017

0.004 0.005 0.007

0.003 0.005 0.006

0.041 0.037 0.031

0.0005 0.0005 0.0011

0.004 0.005 0.0024 48.0

0.005 0.005 0.0026 52.0

0.050 0.037 0.0048 13.0

sr =Repeatability std dev 0.0006 0.0005 0.0011

0.0000 0.0000 0.0007

Page 22

0.0005 0.0008 0.0008

CONSISTENCY BETWEEN LABS h = (lab avg - interlab avg) / std dev of lab avgs Low Al Med Al High Al 2.50 2.31 -1.46 -0.42 0.00 1.04 -0.83 -0.38 -0.21 0.00 -0.38 -0.42 0.00 # 0.00 -0.38 0.83 0.00 0.00 0.21 -0.42 -0.77 -0.42 -0.83 -0.77 0.83 0.42 0.00 0.42 -0.42 -0.77 -0.83 -0.42 -0.77 -0.21 -0.42 -0.38 0.21 -0.42 -0.77 0.21 0.83 0.77 0.42 1.25 1.15 -0.42 0.00 -0.38 -0.63 # # -0.83 0.42 0.00 0.21 0.00 -0.38 0.21 0.42 0.00 0.83 -0.83 -1.15 -0.42 -1.67 -1.54 0.21 3.33 h 3.08 h -1.25 0.00 -0.38 0.42 -0.42 -0.77 1.25 0.83 0.77 -1.46 -1.25 -1.54 3.54 -0.42 0.00 -1.04 # # -0.42 -0.77 0.83 0.00 0.00 0.00 0.83 0.38 -1.25 # # # # # # # # # # # # # # # # # # # # # # # # # # # #

|h| >2.64 indicates statistically significant variation between

31 labs.

#

h #

# # # # # # # # # # # # # #

CONSISTENCY WITHIN LAB k = lab std dev / repeatability std dev Low Al Med Al High Al 0.00 0.00 0.36 0.00 1.00 0.82 0.83 0.80 1.00 0.00 0.00 0.36 0.67 # # 0.67 0.80 0.36 1.33 1.00 1.64 0.00 1.00 0.36 0.83 0.00 0.45 0.00 1.00 1.27 1.00 2.20 k 2.45 k 0.83 0.80 0.36 0.00 1.00 0.45 0.00 0.00 0.36 0.83 1.60 1.00 0.67 1.80 0.36 0.67 0.00 0.36 # # 0.45 0.67 0.00 0.73 0.83 0.80 2.27 k 2.67 k 1.80 0.73 0.83 1.40 0.91 0.00 0.00 2.18 k 0.00 0.80 0.36 0.00 0.00 0.00 0.00 0.00 1.00 0.67 0.00 0.36 3.50 k 2.40 k 0.91 0.83 1.00 1.55 # # # 0.83 0.00 0.45 0.83 0.00 0.73 1.83 1.40 0.73 # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # # #

k > 1.89 indicates statistically significant variation within lab for 31 labs, 5 replicates.


INTERLAB SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. Al 0.014 0.012 0.01

% Al

0.008 0.006 0.004 0.002 0

1

3

5

7

9

11

13

15

Avg = 0.005%

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab Number

Medium Conc. Al 0.014 0.012 0.01

% Al

0.008 0.006 0.004 0.002 0

1

3

5

7

9

11

13

15

Avg = 0.005%

17

19

Lab Number

High Conc. Al 0.06 0.05

% Al

0.04 0.03 0.02 0.01 0

1

3

Avg = 0.037%

5

7

9

11

13

15

17

19

21

23

25

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of test results.

27

29

31

33


TABLE 10

ICRI REPORT NO 641 4/9/13

INTERLAB SPECTROMETER PROFICIENCY TESTING CERIUM

AVERAGE STANDARD DEVIATION Low Ce Med Ce High Ce Low Ce Med Ce High Ce 0.001 0.001 0.001 0.0000 0.0000 0.0000

Lab Lab 1 Lab 2 Lab 3 Lab 4 Lab 5 Lab 6 Lab 7 Lab 8 Lab 9 Lab 10 Lab 11 Lab 12 Lab 13 Lab 14 Lab 15 Lab 16 Lab 17 Lab 18 Lab 19 Lab 20 Lab 21 Lab 22 Lab 23 Lab 24 Lab 25 Lab 26 Lab 27 Lab 28 Lab 29 Lab 30 Lab 31 Lab 32 Lab 33

0.007

0.006

0.003

0.0028

0.0058

0.0028

0.003 0.005

0.004 0.004

0.008 0.009

0.0007 0.0008

0.0004 0.0010

0.0004 0.0018

0.002 0.006

0.0004

0.002

Target Interlab Avg Std Dev of Avg Coef of variation

0.003 0.001

0.005

0.003 0.001 0.004 0.004 0.001

0.002 0.001 0.003 0.002 0.001

0.012 0.003 0.004 0.006 0.002 0.007 0.003 0.002

0.003 0.003

0.001 0.004

0.003 0.009 0.028 0.005

0.0000 0.0008

0.0024 0.0006

0.0013

0.0004

0.0000

0.0004 0.0009 0.0000

0.0000 0.0011 0.0004

0.0007 0.0004 0.0000 0.0005 0.0007 0.0008 0.0004 0.0004

0.001 0.001 0.006

0.0007 0.0005

0.0000 0.0007

0.0005 0.0006 0.0017

0.003 0.010

0.003 0.010

0.0050

0.0100

0.0000 0.0039

0.029 0.004

0.031 0.004

0.0013 0.0004

0.0008 0.0008

0.0009 0.0015

0.004 0.010 0.015 0.005 0.005 0.006 0.0062 0.0068 0.0065 124.0 136.0 108.3

sr =Repeatability std dev 0.0017 0.0032 0.0013

Page 24

CONSISTENCY CONSISTENCY BETWEEN LABS WITHIN LAB h = (lab avg - interlab avg) k = lab std dev / std dev of lab avgs / repeatability std dev Low Ce Med Ce High Ce Low Ce Med Ce High Ce -0.65 -0.59 -0.77 0.00 0.00 0.00 ## ## ## ### ## ## ## ## ## ### ## ## 0.32 0.15 -0.46 1.65 1.81 2.15 k ## ## ## ### ## ## -0.32 -0.15 0.31 0.41 0.13 0.31 0.00 -0.15 0.46 0.47 0.31 1.38 ## ## ## ### ## ## ## ## -0.62 ## 0.00 -0.48 ## 0.00 0.24 ## 0.62 ## ## ## ### ## ## -0.32 0.00 0.92 1.41 0.41 0.54 -0.65 ## -0.46 0.35 0.31 ## ## -0.31 ### ## 0.00 -0.32 -0.44 0.00 0.24 0.00 0.38 -0.65 -0.59 -0.62 0.54 -0.16 -0.29 0.15 0.24 0.00 0.62 -0.16 -0.44 -0.46 0.53 0.34 0.31 -0.65 -0.59 -0.62 0.00 0.13 0.31 ## ## ## ### ## ## ## ## ## ### ## ## ## ## -0.77 ### ## 0.38 -0.32 -0.59 -0.77 0.41 0.00 0.46 -0.32 -0.15 0.00 0.29 0.22 1.31 ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## -0.32 -0.29 -0.46 0.00 0.65 0.74 0.62 2.94 k 3.13 k 3.00 k ## ## ## ### ## ## ## ## ## ### ## ## 3.71 h 3.53 h 3.85 h 0.76 0.25 0.69 0.00 -0.15 -0.31 0.24 0.25 1.15 ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ## ## ## ## ### ## ##

|h| >2.57 indicates statistically significant variation between

21 labs.

k > 1.88 indicates statistically significant variation within lab for 21 labs, 5 replicates.


INTERLABORATORY SPECTROMETER PROFICIENCY TESTING

ICRI REPORT NO 641 4/9/13

Low Conc. Ce 0.036

% Ce

0.027

0.018

0.009

0.000

1

3

5

7

9

11

13

15

Avg = 0.005%

17

19

21

23

25

27

29

31

33

21

23

25

27

29

31

33

21

23

25

27

29

31

33

Lab Number

Medium Conc. Ce 0.035 0.030 0.025

% Ce

0.020 0.015 0.010 0.005 0.000

1

3

5

7

9

11

13

15

17

19

Lab Number

Avg = 0.005%

High Conc. Ce 0.035 0.030 0.025

% Ce

0.020 0.015 0.010 0.005 0.000

1

3

Avg = 0.006%

5

7

9

11

13

15

17

19

Lab Number

Note: Actual test results are shown on graph with each lab average offset to the right of the test results.


ICRI REPORT NO. 641 4/9/13

APPENDIX I Calculation of statistics used to measure the precision of a test method. The standard deviation is calculated in the classical manner by the following formula.

where x = the individual test result 0 = the average of n = 5 test results The h statistic is a measure of reproducibility or consistency between labs

where d = the deviation of the test result average from the average of the test result averages, d = 0 - x=

where p = number of labs or s0 = standard deviation of the test result averages The k statistic is a measure of the repeatability or consistency within a lab. k = s/sr where s = test result standard deviation for one lab sr = the repeatability standard deviation and is the larger of

or

See ASTM E691-05 for a more complete explanation and derivation of equations. Page 26


ICRI REPORT NO. 641 4/9/13 APPENDIX II Participants in Interlaboratory Study - Round 32

Plant Grede-New Castle

ContacW Jim Cree

Weil McLain

Cheryl Cichowlaz

Wescast TDC Wescast-Wingham

Feila Yu Brent Black

Grede-Reedsburg

Mike Rothwell

Neenah Foundry

Phil Kubichka

Neenah Foundry

Phil Kubichka

OSCO-Portsmouth Gunite Corporation

Jake Hackworth Tony Clark

Aarrowcast Grede-Brewton

Cesar Braga Randy Hunt

Glidewell

Brian Richey

Motor Castings Elyria Foundry Hodge Foundry

Stan Hemenway Richard Lewis John McGoldrick

Anderson Labs Dalton-Warsaw Grede-Iron Mtn.

Greg Mann Jeff Drury Greg Jarski

Bremen Castings Rochester Metals Spectro Grede-Columbiana Quality Castings Grede-St. Cloud A

Matt Meyer Matt Calcutt Calvin Simon John Nicholas Rob Schmidt

Benton Foundry John Deere Foundry C.A. Lawton

Keith Provine Ashley Assink Rob Christensen

Casting Solutions LLC OSCO-Jackson Gunite Corporation

Art Boehme Chris Maness Tony Clark

Tyco

Don Perry

ACIPCO OSCO-New Boston Rochester Metals WAS

Don Denney Tom Brower Matt Calcutt

6SHFWURPHWHU Brand ARL ARL

Spectrometer Model 2460

ARL ARL ARL

Software Win OE Ver. 2.2-1

Burns 2-3

3460

Win OE 2.12

3

3460 3460

WinOE version 3.2-2 WIN OE 3.2-2

2 2-3

4460

ARL

2

ARL #1 ARL #2

4460

Win OE 2.1-3

2

4460

Win OE 2.1-3

2

ARL

Metals Analyzer DV-6

Win OE 3.0.1 ?

2 1

Q6 Columbus Quantron Magellen

Qmatrix QMatrix

2 2

GDS 500

GDS 500A Software v1.61

2

GDS 500 A GDS 500A GDS 750

GDS500A Ver. 1.50 GDS 500A Software v1.50 Bulk Analysis v 4.5.3

2 3 2

GDS SA-2000 LAV X9 LAVFA18B

LECO 4.60 Spark Analyzer Vision Spectro 1.32a

3 2 2

LAVMB08B LAVMB08B LAVMB18B MAXx SpectroLab F

Spectro Ver 1.32 V4.23d Spectro Metal Prog. 4.20d GSPC Spectro Ver. 3.0

2 2 2-3 2 2-3

SpectroLab SpectroLab M9 SpectroMAXx

Windows NT Spark Analyzer Vision 1.51 MX 1.00.0011

2-4 3 2

SpectroMAXx SpectroMAXx SpectroMAXx F

Spark Analyzer MX Ver. 1.27 Spark Analyzer Vision Mx Spark Analyzer Vision Mx 1.00.0011

2-3 2 2

Baird Bruker Bruker LECO LECO LECO LECO LECO Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro Spectro WAS

SpectroMAXx F

DIA

2

SpectroMaXx LMF15 SpectroMAXx MBT LMX05 Foundrymaster

Spark Analyzer Vision MX V. 1.0 Spark Analyzer Vision MX Foundry Master V3.08c

3 2 2

Page 27


ICRI REPORT NO. 641 4/9/13

Appendix III Recent History of h and k Occurrences Above Critical Round 32 Lab Round 32 Round 31 Round 30 Round 29 Round 28 Round 27 Round 26 Round 25 h&k Numbers h&k h&k h&k h&k h&k h&k h&k 1 1 0 2 0 3 1 2 . 2 0 1 0 0 0 0 0 0 3 0 0 0 0 0 0 0 0 4 3 4 1 1 4 9 7 7 5 0 0 0 1 0 0 . . 6 0 0 0 0 1 2 0 0 1 0 0 1 4 6 8 1 7 8 0 0 0 2 7 . . . 9 0 0 0 0 4 6 7 2 10 0 0 0 5 5 2 2 . 11 14 7 2 5 1 2 0 8 12 1 1 3 1 4 0 1 0 13 0 0 2 0 2 3 1 4 14 2 0 1 1 0 0 0 4 15 4 0 0 0 0 2 2 1 16 2 4 1 2 . . . . 17 1 0 0 0 0 2 1 2 18 0 0 0 0 1 2 1 3 19 0 . . . . . . . 20 4 2 9 8 1 4 5 4 21 3 0 2 1 0 0 . . 22 0 12 10 6 . . . 23 5 10 0 3 0 1 6 . 24 3 0 1 2 1 3 1 . 25 0 0 0 0 0 0 0 0 26 0 0 1 0 3 5 1 0 27 5 3 0 0 . 0 . 2 28 9 2 0 . 1 1 . 29 10 9 13 0 6 2 . 4 30 11 13 14 . . . . . 31 1 . . . . . . . 32 4 2 2 3 6 2 4 4 33 4 0 0 0 . . . .

Page 28


This information, or parts of it may not be published or divulged without prior written permission from the Institute. Iron Casting Research Institute, 2802 Fisher Road, Columbus, Ohio

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Rpt 641 spectresultsround32