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CEMENT AND CONCRETE REFERENCE LABORATORY PROFICIENCY SAMPLE PROGRAM Final Report Portland Cement Proficiency Samples Number 203 and Number 204 March 2017 www.ccrl.us

www.ccrl.us March 15, 2017 TO: Participants in the CCRL Portland Cement Proficiency Sample Program SUBJECT: Final Report on Portland Cement Proficiency Samples No. 203 and No. 204 Following is the final report for the current pair of CCRL Portland Cement Proficiency Samples which were distributed in January 2017. Portland Cement Samples No. 203 was an ASTM C150 meeting the specifications of Type I and contained a limestone addition. Portland Cement No. 204 was an ASTM C150 meeting the specifications of Type I and Type II, and contained a limestone addition. This report consists of a statistical Summary of Results, a set of general Scatter Diagrams, and associated detailed information. The Table of Results with individualized information for participating laboratories can be downloaded at our website located at:http://www.ccrl.us/. Additional information is provided in the following pages. An informational summary on Air Jet Sieve Study is found on the following page. The CCRL Proficiency Sample Programs are intended for internal use by the laboratory as a tool to identify potential problems in laboratory procedures or test equipment and to initiate remedial actions. These programs are designed to complement the CCRL Laboratory Inspection Program as part of a total quality system. Care should be taken when using this program for any other purpose. Additional samples of these two cements and other CCRL samples are available for purchase. These samples may be useful for equipment verification, technician training, and research. Contact CCRL for availability and price. It is presently anticipated that the next Portland Cement Proficiency Samples will be distributed in June 2017. Sincerely, Robin K. Haupt Supervisor, Proficiency Sample Programs Cement and Concrete Reference Laboratory 4441 Buckeystown Pike, Suite C Frederick, Maryland 21704 phone: 240-436-4800 fax: 610-834-7066 email: ccrl@astm.org Sponsored by Committees C-1 and C-9 of ASTM International

CCRL Portland Cement Samples No. 203 & No. 204 Informational Summary Air Jet Sieve Study For this set of CCRL Portland Cement Samples, ASTM C01.25 Subcommittee requested laboratories perform 45µm sieve fineness using air jet sieve apparatus. Results were reported by 44 laboratories. These results have been provided to the Subcommittee for their evaluation. Below is an informational summary of these results. Minimum value reported Maximum value reported Average Standard deviation Vacuum pressure, kpa 1.0 10.0 4.4 Time, seconds 30 300 184 Sieve correction factor 31.0 73.6 13.7 Sample 203 All data Corrected % passing 76.7 98.9 95.2 3.1 Sample 204 All Data Corrected % passing 64.3 99.5 96.4 5.1 Sample 203 Outlying data removed Corrected % passing 91.7 98.9 95.7 1.2 Sample 204 Outlying data removed Corrected % passing 91.7 99.5 97.1 1.1 Sieve Calibration Standard used (number reported using) SRM 46h 18 Internal secondary 13 standard SRM 114 12 None reported 1

TO: Participants in the CCRL Portland Cement Proficiency Sample Program FROM: Robin K. Haupt, Supervisor PSP SUBJECT: Explanation of Final Report on Results of Tests for Portland Cement Proficiency Samples No. 203 and No. 204 This letter, and the material included with it, constitutes the final report, and summary of results for the current pair of Portland Cement Proficiency Samples, which were distributed in January 2017. This material includes a Table of Results for individual laboratory data, a statistical Summary of Results, and a set of general Scatter Diagrams. Your unique laboratory number is displayed at the top of the individual Table of Results. An explanation of the program is contained in the paper: "Statistical Evaluation of Interlaboratory Cement Tests" by J. R. Crandall and R. L. Blaine View Document, and "Statistical Aspects of the Cement Testing Program" by W.J. Youden View Document, which can be found in Volume 59, Proceedings of the 62 nd Annual Meeting of the Society, June 25, 1959, American Society for Testing and Materials. Each laboratory receives an individualized Table of Results. The Table of Results shows the, test title, and the reporting unit in the first two columns. After that it lists in order, the laboratory's results for the odd and even numbered samples, overall averages for the odd and even numbered samples, and the laboratory's ratings for the odd and even samples. Laboratory ratings, shown in the Table of Results for the individual laboratory, were determined in the manner described by Crandall and Blaine using a rating scale of 1 to 5 instead of 0 to 4. The ratings have no valid standing beyond showing the difference between the individual laboratory result and the average for a particular test. The following table details the relationship between the ratings and the averages. Ratings Range (Number of Number (Per 100) Standard Deviations) of Laboratories achieving the rating 1 5 Less than 1 69 4 1 to 1.5 18 3 1.5 to 2 9 2 2 to 2.5 3 1 Greater than 2.5 1 The sign of the rating merely shows whether the result reported was greater or less than the average obtained. Participants subscribing to the primary chemical analysis portion of this report should note that the statistics were calculated using data obtained by wet methods, and rapid methods of chemical analysis. Participants in the secondary chemical analysis should note that laboratory ratings are assigned using primary chemical statistics. Please note that individual laboratory ratings were not given for the flow of air content mortar (test no. 190) and compressive strength mortar (test no. 230). Air content flows in the range of 87.5 ± 7.5 are satisfactory; labs with flow values outside this range will be flagged as a Labs Eliminated or Labs Off Diagram on the scatter diagram. Averages, standard deviations, and a scatter diagram are provided for your information. This information may be a helpful indicator of a problem with flow table apparatus or mortar mixing 1 Youden, W.J., Statistical Aspects of the Cement Testing Program,Volume 59, Proceedings of the 62 nd Annual Meeting of the Society, June 25, 1959, American Society for Testing and Materials. Explanation of Final Report - page 1 of 2

procedures. Flow values of 151 were assigned to laboratories reporting a mortar flow off the flow table top. In cases where some laboratories' results are eliminated, averages, standard deviations, coefficients of variation, and the ratings of the other laboratories' results, are recalculated using the data remaining after the elimination. Since the laboratory ratings given are the results from this one series of tests, you need not attach too much significance to a single low rating, or pair of ratings, from this one series. A continuing tendency to get low ratings on several pairs of samples should lead a laboratory to consider the types of error, systematic and random, contribute to ratings that are low. Systematic error, which is indicated by low ratings with the same signs on each pair of samples, means a consistent error is occurring in equipment and/or test procedures. One indication of random error is low ratings on both samples with different signs. Since systematic error occurs with more regularity, its cause is generally easier to find than the cause of random error. Summary of Results Usually, averages, standard deviations, and coefficients of variation are given with all results reported, and then with one or more outlying results omitted. Sometimes, two or more recalculations with laboratories omitted, have been done for the same test. In these cases, all of the laboratories omitted in previous recalculations are also omitted in subsequent ones. Results omitted are values that are more than three standard deviations from the mean of one or both samples. Often, elimination of these outlying results has little effect on the average, but may have a more pronounced effect on the standard deviation and coefficient of variation. Scatter Diagrams General scatter diagrams are supplied with this report. Crandall and Blaine describe the manner of preparing scatter diagrams, and their interpretation, in the paper published in the 1959 ASTM Proceedings. Each laboratory will receive a complete set of diagrams according to their subscription to the given program. Using the results received from each laboratory, a scatter diagram is generated for each test method by plotting the value for the odd numbered samples on the X, or horizontal axis, against the value for the even numbered samples on the Y, or vertical axis. To find your point, just plot as you would when plotting any scatter diagram. Vertical and horizontal dashed lines, which divide the diagrams into four sections or quadrants, place the average values for the odd and even numbered samples, respectively. The first line of print under the diagram includes the test number, as given on the data sheet, the test title, and the number of data points on the diagrams. The number of plotted points may not agree with the total number of data pairs included in the analysis because a few points may be off the diagram, and some points may represent several data pairs, which are identical. Laboratories whose points are off the diagram will have a rating of ±1 for that particular test. As described in Crandall and Blaine, a tight circular pattern of points around the intersection of the median lines is the ideal situation. Stretching out of the pattern into the first (upper right) and third (lower left) quadrants, suggests some kind of bias, or tendency for laboratories to get high or low results on both samples. Examination of the scatter diagrams indicates strong evidence of bias on many tests. Explanation of Final Report - page 2 of 2

CCRL PROFICIENCY SAMPLE PROGRAM Portland Cement Proficiency Samples No. 203 and No. 204 Final Report Primary Chemical Results March 15, 2017 SUMMARY OF RESULTS Sample No.203 Test (unit) #Labs Average S.D. C.V. Average S.D. C.V. Silicon Dioxide (percent) 232 19.48 0.20 1.05 19.67 1.11 5.62 *224 19.48 0.16 0.82 19.75 0.18 0.91 * Labs Eliminated - 48, 50, 95, 98, 284, 684, 1644, 4142 Aluminum Oxide (percent) 229 4.96 0.13 2.6 4.20 0.11 2.6 *218 4.96 0.08 1.6 4.18 0.08 1.8 * Labs Eliminated - 14, 42, 50, 134, 157, 698, 1956, 2477, 4099, 4137, 4206 Ferric Oxide (percent) 229 3.85 0.08 2.0 3.45 0.07 1.9 *216 3.86 0.04 1.1 3.45 0.04 1.2 * Labs Eliminated - 22, 126, 134, 162, 206, 416, 2477, 2491, 4051, 4080, 4099, 4150, 4206 Calcium Oxide (percent) 229 63.27 0.42 0.66 62.72 0.49 0.78 *226 63.30 0.34 0.54 62.74 0.47 0.75 * Labs Eliminated - 98, 284, 4206 Magnesium Oxide (percent) 230 1.17 0.20 16.8 3.09 0.22 7.2 *219 1.15 0.05 4.0 3.11 0.09 2.8 * Labs Eliminated - 14, 84, 134, 206, 222, 493, 779, 2463, 2477, 4039, 4099 Sulfur Trioxide (percent) 233 3.31 0.10 2.9 2.56 0.10 3.8 *219 3.32 0.06 1.9 2.56 0.06 2.4 * Labs Eliminated - 93, 134, 146, 159, 169, 203, 246, 694, 883, 2360, 2463, 3279, 3297, 4142 Loss on Ignition (percent) 236 2.71 0.15 5.4 3.42 0.18 5.1 *221 2.71 0.08 2.9 3.43 0.08 2.3 * Labs Eliminated - 4, 47, 95, 131, 137, 159, 493, 1054, 1644, 1799, 1942, 1956, 3368, 4080, 4099 Summary of Results page 1 of 4

CCRL PROFICIENCY SAMPLE PROGRAM Portland Cement Proficiency Samples No. 203 and No. 204 Final Report Primary Chemical Results March 15, 2017 SUMMARY OF RESULTS Sample No.203 Test (unit) #Labs Average S.D. C.V. Average S.D. C.V. Sodium Oxide (percent) 220 0.070 0.051 73 0.113 0.047 41 *207 0.064 0.020 32 0.110 0.021 19 * Labs Eliminated - 86, 94, 99, 134, 221, 284, 494, 1054, 1644, 2352, 2463, 3368, 4099 Potassium Oxide (percent) 225 0.674 0.024 3.5 0.730 0.029 4.0 *212 0.675 0.015 2.2 0.733 0.018 2.4 * Labs Eliminated - 47, 95, 125, 134, 246, 694, 1956, 2308, 2412, 4080, 4099, 4137, 4206 Strontium Oxide (percent) 112 0.115 0.020 18 0.036 0.011 30 *103 0.120 0.006 5 0.036 0.004 10 * Labs Eliminated - 7, 34, 134, 493, 1657, 2293, 2491, 4099, 4137 Titanium Dioxide (percent) 182 0.26 0.110 42.1 0.26 0.108 41.5 *173 0.25 0.008 3.3 0.25 0.008 3.2 * Labs Eliminated - 175, 246, 493, 1054, 1644, 3707, 4099, 4131, 4137 Phosphorus Pentoxide (percent) 177 0.160 0.037 22.8 0.067 0.028 41.7 *156 0.159 0.006 3.5 0.064 0.005 7.9 * Labs Eliminated - 8, 47, 48, 78, 90, 134, 247, 407, 493, 494, 1799, 2463, 2477, 2483, 2490, 2491, 2522, 4093, 4099, 4115, 4131 Zinc Oxide (percent) 110 0.014 0.014 97.3 0.013 0.011 90.4 *100 0.012 0.002 12.7 0.011 0.001 12.7 * Labs Eliminated - 19, 101, 440, 493, 2462, 2477, 2483, 2491, 2522, 4099 Summary of Results page 2 of 4

CCRL PROFICIENCY SAMPLE PROGRAM Portland Cement Proficiency Samples No. 203 and No. 204 Final Report Primary Chemical Results March 15, 2017 SUMMARY OF RESULTS Sample No.203 Test (unit) #Labs Average S.D. C.V. Average S.D. C.V. Manganic Oxide (percent) 151 0.154 0.022 14.3 0.063 0.017 26.6 *131 0.157 0.005 3.5 0.061 0.004 6.4 * Labs Eliminated - 47, 84, 134, 137, 203, 284, 354, 493, 768, 2293, 2463, 2466, 2477, 2484, 2491, 3238, 3297, 3707, 4099, 4131 Chloride (percent) 138 0.006 0.007 119 0.010 0.009 91 *130 0.005 0.003 67 0.008 0.004 49 * Labs Eliminated - 60, 219, 692, 1644, 1942, 2491, 3057, 3607 Insoluble Residue (percent) 220 0.39 0.17 43 0.58 0.16 28 *204 0.36 0.09 25 0.56 0.10 18 * Labs Eliminated - 8, 24, 26, 36, 159, 206, 209, 246, 493, 768, 2465, 3249, 3368, 3658, 4155, 4200 Free Lime (percent) 181 1.58 0.32 20 1.27 0.28 22 *174 1.62 0.25 15 1.29 0.25 19 * Labs Eliminated - 126, 415, 450, 768, 881, 3297, 4206 Carbon Dioxide (percent) 206 1.81 0.32 17.7 2.51 0.38 15.2 *190 1.84 0.18 10.0 2.57 0.17 6.7 * Labs Eliminated - 129, 137, 142, 169, 206, 415, 416, 457, 1054, 2490, 3607, 4051, 4093, 4150, 4155, 4206 Limestone Content (percent) 202 4.5 0.8 17.3 5.9 0.9 15.4 *188 4.6 0.5 11.0 6.1 0.5 7.7 * Labs Eliminated - 129, 137, 142, 169, 206, 219, 415, 457, 886, 1435, 4051, 4093, 4150, 4155 Summary of Results page 3 of 4

CCRL PROFICIENCY SAMPLE PROGRAM Portland Cement Proficiency Samples No. 203 and No. 204 Final Report Primary Chemical Results March 15, 2017 SUMMARY OF RESULTS Sample No.203 Test (unit) #Labs Average S.D. C.V. Average S.D. C.V. Chromium Oxide (percent) 101 0.012 0.010 87 0.010 0.007 65 *82 0.009 0.002 19 0.009 0.002 17 * Labs Eliminated - 34, 36, 66, 105, 116, 157, 415, 438, 493, 1079, 1466, 2462, 2491, 2522, 3057, 3238, 3279, 3368, 4099 Tricalcium Silicate (percent) 200 54.5 3.7 6.8 56.8 4.1 7.2 *197 54.6 3.3 6.1 56.8 3.9 6.8 * Labs Eliminated - 206, 1942, 4206 Dicalcium Silicate (percent) 200 14.3 3.1 21.9 13.0 3.1 24.1 *196 14.3 2.8 19.4 13.0 2.9 22.0 * Labs Eliminated - 137, 206, 1942, 4206 Tricalcium Aluminate (percent) 200 6.6 0.4 5.8 5.1 0.5 8.8 *195 6.6 0.2 3.6 5.1 0.2 4.8 * Labs Eliminated - 134, 494, 2477, 3238, 4137 Tetracalcium Aluminoferrite (percent) 200 11.6 0.3 2.6 10.5 0.7 6.6 *195 11.6 0.2 2.0 10.4 0.2 2.2 * Labs Eliminated - 134, 438, 494, 2477, 3238 Summary of Results page 4 of 4

Silicon Dioxide 20.30 20.20 20.10 20.00 Silicon Dioxide (percent) 19.90 19.80 19.70 19.60 19.50 19.40 19.30 19.20 18.90 19.00 19.10 19.20 19.30 19.40 19.50 19.60 19.70 19.80 19.90 20.00 Silicon Dioxide (percent) Test No. 10 Silicon Dioxide 220 Points Ave 19.48 S.D. 0.16 C.V. 0.82 Ave 19.75 S.D. 0.18 C.V. 0.91 Labs Eliminated: 48, 50, 95, 98, 284, 684, 1644, 4142 Labs off Diagram: 134, 2437, 2477, 3297

Aluminum Oxide 4.40 4.30 Aluminum Oxide (percent) 4.20 4.10 4.00 4 3.90 4.70 4.80 4.90 5.00 5 5.10 5.20 Aluminum Oxide (percent) Test No. 21 Aluminum Oxide 218 Points Ave 4.96 S.D. 0.08 C.V. 1.6 Ave 4.18 S.D. 0.08 C.V. 1.8 Labs Eliminated: 14, 42, 50, 134, 157, 698, 1956, 2477, 4099, 4137, 4206

Ferric Oxide 3.60 3.55 Ferric Oxide (percent) 3.50 3.45 3.40 3.35 3.30 3.70 3.75 3.80 3.85 3.90 3.95 4.00 4 Ferric Oxide (percent) Test No. 30 Ferric Oxide 216 Points Ave 3.86 S.D. 0.04 C.V. 1.1 Ave 3.45 S.D. 0.04 C.V. 1.2 Labs Eliminated: 22, 126, 134, 162, 206, 416, 2477, 2491, 4051, 4080, 4099, 4150, 4206

Calcium Oxide 64.50 64.00 63.50 Calcium Oxide (percent) 63.00 62.50 62.00 61.50 61.00 61.50 62.00 62.50 63.00 63.50 64.00 64.50 65.00 Calcium Oxide (percent) Test No. 40 Calcium Oxide 226 Points Ave 63.30 S.D. 0.34 C.V. 0.54 Ave 62.74 S.D. 0.47 C.V. 0.75 Labs Eliminated: 98, 284, 4206

Magnesium Oxide 3.45 3.40 3.35 3.30 Magnesium Oxide (percent) 3.25 3.20 3.15 3.10 3.05 3.00 3 2.95 2.90 2.85 2.80 0.80 0.85 0.90 0.95 1.00 1 1.05 1.10 1.15 1.20 1.25 1.30 1.35 1.40 1.45 Magnesium Oxide (percent) Test No. 50 Magnesium Oxide 219 Points Ave 1.15 S.D. 0.05 C.V. 4.0 Ave 3.11 S.D. 0.09 C.V. 2.8 Labs Eliminated: 14, 84, 134, 206, 222, 493, 779, 2463, 2477, 4039, 4099

Sulfur Trioxide 2.75 2.70 2.65 Sulfur Trioxide (percent) 2.60 2.55 2.50 2.45 2.40 2.35 2.30 3.10 3.15 3.20 3.25 3.30 3.35 3.40 3.45 3.50 3.55 Sulfur Trioxide (percent) Test No. 60 Sulfur Trioxide 219 Points Ave 3.32 S.D. 0.06 C.V. 1.9 Ave 2.56 S.D. 0.06 C.V. 2.4 Labs Eliminated: 93, 134, 146, 159, 169, 203, 246, 694, 883, 2360, 2463, 3279, 3297, 4142

Loss on Ignition 3.70 3.60 Loss on Ignition (percent) 3.50 3.40 3.30 3.20 3.10 2.40 2.50 2.60 2.70 2.80 2.90 3.00 3 Loss on Ignition (percent) Test No. 70 Loss on Ignition 221 Points Ave 2.71 S.D. 0.08 C.V. 2.9 Ave 3.43 S.D. 0.08 C.V. 2.3 Labs Eliminated: 4, 47, 95, 131, 137, 159, 493, 1054, 1644, 1799, 1942, 1956, 3368, 4080, 4099

Sodium Oxide 0.160 0.140 Sodium Oxide (percent) 0.120 0.100 0.080 0.060 0.040 0.0000 0.020 0.040 0.060 0.080 0.100 0.120 Sodium Oxide (percent) Test No. 90 Sodium Oxide 204 Points Ave 0.064 S.D. 0.020 C.V. 32 Ave 0.110 S.D. 0.021 C.V. 19 Labs Eliminated: 86, 94, 99, 134, 221, 284, 494, 1054, 1644, 2352, 2463, 3368, 4099 Labs off Diagram: 41, 416, 3607

Potassium Oxide 0.780 0.760 Potassium Oxide (percent) 0.740 0.720 0.700 0.680 0.620 0.640 0.660 0.680 0.700 0.720 Potassium Oxide (percent) Test No. 100 Potassium Oxide 212 Points Ave 0.675 S.D. 0.015 C.V. 2.2 Ave 0.733 S.D. 0.018 C.V. 2.4 Labs Eliminated: 47, 95, 125, 134, 246, 694, 1956, 2308, 2412, 4080, 4099, 4137, 4206

Strontium Oxide 0.055 0.050 0.045 Strontium Oxide (percent) 0.040 0.035 0.030 0.025 0.020 0.015 0.010 0.100 0.105 0.110 0.115 0.120 0.125 0.130 0.135 0.140 0.145 Strontium Oxide (percent) Test No. 92 Strontium Oxide 103 Points Ave 0.120 S.D. 0.006 C.V. 5 Ave 0.036 S.D. 0.004 C.V. 10 Labs Eliminated: 7, 34, 134, 493, 1657, 2293, 2491, 4099, 4137

Titanium Dioxide 0.28 0.27 Titanium Dioxide (percent) 0.26 0.25 0.24 0.23 0.22 0.22 0.23 0.24 0.25 0.26 0.27 0.28 Titanium Dioxide (percent) Test No. 103 Titanium Dioxide 173 Points Ave 0.25 S.D. 0.008 C.V. 3.3 Ave 0.25 S.D. 0.008 C.V. 3.2 Labs Eliminated: 175, 246, 493, 1054, 1644, 3707, 4099, 4131, 4137

Phosphorus Pentoxide 0.080 0.075 0.070 Phosphorus Pentoxide (percent) 0.065 0.060 0.055 0.050 0.045 0.040 0.140 0.145 0.150 0.155 0.160 0.165 0.170 0.175 0.180 Phosphorus Pentoxide (percent) Test No. 102 Phosphorus Pentoxide 154 Points Ave 0.159 S.D. 0.006 C.V. 3.5 Ave 0.064 S.D. 0.005 C.V. 7.9 Labs Eliminated: 8, 47, 48, 78, 90, 134, 247, 407, 493, 494, 1799, 2463, 2477, 2483, 2490, 2491, 2522, 4093, 4099, 4115, 4131 Labs off Diagram: 60, 413

Zinc Oxide 0.015 0.014 0.013 Zinc Oxide (percent) 0.012 0.011 0.010 0.009 0.008 0.007 0.006 0.007 0.008 0.009 0.010 0.011 0.012 0.013 0.014 0.015 0.016 Zinc Oxide (percent) Test No. 99 Zinc Oxide 100 Points Ave 0.012 S.D. 0.002 C.V. 12.7 Ave 0.011 S.D. 0.001 C.V. 12.7 Labs Eliminated: 19, 101, 440, 493, 2462, 2477, 2483, 2491, 2522, 4099

Manganic Oxide 0.075 0.070 Manganic Oxide (percent) 0.065 0.060 0.055 0.050 0.045 0.040 0.140 0.145 0.150 0.155 0.160 0.165 0.170 0.175 Manganic Oxide (percent) Test No. 101 Manganic Oxide 131 Points Ave 0.157 S.D. 0.005 C.V. 3.5 Ave 0.061 S.D. 0.004 C.V. 6.4 Labs Eliminated: 47, 84, 134, 137, 203, 284, 354, 493, 768, 2293, 2463, 2466, 2477, 2484, 2491, 3238, 3297, 3707, 4099, 4131

Chloride 0.020 0.015 Chloride (percent) 0.010 0.005 0.000 0-0.005-0.010-0.005 0.0000 0.005 0.010 0.015 Chloride (percent) Test No. 104 Chloride 130 Points Ave 0.005 S.D. 0.003 C.V. 67 Ave 0.008 S.D. 0.004 C.V. 49 Labs Eliminated: 60, 219, 692, 1644, 1942, 2491, 3057, 3607

Insoluble Residue 0.90 0.85 0.80 0.75 Insoluble Residue (percent) 0.70 0.65 0.60 0.55 0.50 0.45 0.40 0.35 0.30 0.25 0.20 0.00 0 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 Insoluble Residue (percent) Test No. 80 Insoluble Residue 204 Points Ave 0.36 S.D. 0.09 C.V. 25 Ave 0.56 S.D. 0.10 C.V. 18 Labs Eliminated: 8, 24, 26, 36, 159, 206, 209, 246, 493, 768, 2465, 3249, 3368, 3658, 4155, 4200

Free Lime 2.10 1.90 1.70 Free Lime (percent) 1.50 1.30 1.10 0.90 0.70 0.50 0.80 1.00 1 1.20 1.40 1.60 1.80 2.00 2 2.20 2.40 Free Lime (percent) Test No. 41 Free Lime 174 Points Ave 1.62 S.D. 0.25 C.V. 15 Ave 1.29 S.D. 0.25 C.V. 19 Labs Eliminated: 126, 415, 450, 768, 881, 3297, 4206

Carbon Dioxide 3.20 3.10 3.00 3 2.90 Carbon Dioxide (percent) 2.80 2.70 2.60 2.50 2.40 2.30 2.20 2.10 2.00 2 1.20 1.30 1.40 1.50 1.60 1.70 1.80 1.90 2.00 2 2.10 2.20 2.30 2.40 Carbon Dioxide (percent) Test No. 97 Carbon Dioxide 189 Points Ave 1.84 S.D. 0.18 C.V. 10.0 Ave 2.57 S.D. 0.17 C.V. 6.7 Labs Eliminated: 129, 137, 142, 169, 206, 415, 416, 457, 1054, 2490, 3607, 4051, 4093, 4150, 4155, 4206 Labs off Diagram: 247

Limestone Content 7.5 7.0 7 Limestone Content (percent) 6.5 6.0 6 5.5 5.0 5 4.5 4.0 4 3.0 3 3.5 4.0 4 4.5 5.0 5 5.5 6.0 6 6.5 Limestone Content (percent) Test No. 98 Limestone Content 187 Points Ave 4.6 S.D. 0.5 C.V. 11.0 Ave 6.1 S.D. 0.5 C.V. 7.7 Labs Eliminated: 129, 137, 142, 169, 206, 219, 415, 457, 886, 1435, 4051, 4093, 4150, 4155 Labs off Diagram: 4206

Chromium Oxide 0.014 0.012 Chromium Oxide (percent) 0.010 0.008 0.006 0.004 0.004 0.006 0.008 0.010 0.012 0.014 Chromium Oxide (percent) Test No. 105 Chromium Oxide 82 Points Ave 0.009 S.D. 0.002 C.V. 19 Ave 0.009 S.D. 0.002 C.V. 17 Labs Eliminated: 34, 36, 66, 105, 116, 157, 415, 438, 493, 1079, 1466, 2462, 2491, 2522, 3057, 3238, 3279, 3368, 4099

Tricalcium Silicate 69.0 67.0 65.0 63.0 Tricalcium Silicate (percent) 61.0 59.0 57.0 55.0 53.0 51.0 49.0 47.0 45.0 42.0 44.0 46.0 48.0 50.0 52.0 54.0 56.0 58.0 60.0 62.0 64.0 66.0 Tricalcium Silicate (percent) Test No. 106 Tricalcium Silicate 197 Points Ave 54.6 S.D. 3.3 C.V. 6.1 Ave 56.8 S.D. 3.9 C.V. 6.8 Labs Eliminated: 206, 1942, 4206

Dicalcium Silicate 22.0 20.0 18.0 Dicalcium Silicate (percent) 16.0 14.0 12.0 10.0 8.0 8 6.0 6 4.0 4 5.0 5 7.0 7 9.0 9 11.0 13.0 15.0 17.0 19.0 21.0 23.0 Dicalcium Silicate (percent) Test No. 107 Dicalcium Silicate 196 Points Ave 14.3 S.D. 2.8 C.V. 19.4 Ave 13.0 S.D. 2.9 C.V. 22.0 Labs Eliminated: 137, 206, 1942, 4206

Tricalcium Aluminate 5.8 5.6 Tricalcium Aluminate (percent) 5.4 5.2 5.0 5 4.8 4.6 4.4 5.8 6.0 6 6.2 6.4 6.6 6.8 7.0 7 7.2 Tricalcium Aluminate (percent) Test No. 108 Tricalcium Aluminate 191 Points Ave 6.6 S.D. 0.2 C.V. 3.6 Ave 5.1 S.D. 0.2 C.V. 4.8 Labs Eliminated: 134, 494, 2477, 3238, 4137 Labs off Diagram: 42, 206, 1956, 4206

Tetracalcium Aluminoferrite 11.0 10.8 Tetracalcium Aluminoferrite (percent) 10.6 10.4 10.2 10.0 9.8 9.6 10.8 11.0 11.2 11.4 11.6 11.8 12.0 12.2 Tetracalcium Aluminoferrite (percent) Test No. 109 Tetracalcium Aluminoferrite 193 Points Ave 11.6 S.D. 0.2 C.V. 2.0 Ave 10.4 S.D. 0.2 C.V. 2.2 Labs Eliminated: 134, 438, 494, 2477, 3238 Labs off Diagram: 60, 4051

CCRL PROFICIENCY SAMPLE PROGRAM Portland Cement Proficiency Samples No. 203 and No. 204 Final Report Physical Results March 15, 2017 SUMMARY OF RESULTS Sample No.203 Test (unit) #Labs Average S.D. C.V. Average S.D. C.V. Normal Consistency - % Water (percent) 256 26.3 2.90 11.00 26.6 2.84 10.70 *249 26.4 0.45 1.70 26.7 0.46 1.70 * Labs Eliminated - 497, 557, 2477, 3850, 4080, 4137, 4200 Vicat Time of Set - Initial (minutes) 252 127 13 10 138 13 10 *247 126 12 9 138 12 8 * Labs Eliminated - 1715, 2462, 2477, 4142, 4206 Vicat Time of Set - Final (minutes) 244 222 32 14 242 31 13 *237 219 27 12 240 28 12 * Labs Eliminated - 8, 74, 132, 165, 1466, 3801, 4206 Gillmore Time of Set - Initial (minutes) 144 161 23 14 175 23 13 *141 160 22 14 173 20 11 * Labs Eliminated - 18, 408, 493 Gillmore Time of Set - Final (minutes) 144 254 37 15 276 35 13 *143 254 36 14 275 33 12 * Labs Eliminated - 18 False Set - Paste Method (percent) 191 81 8.0 9.9 79 9.0 11.4 *189 81 8.0 9.9 79 8.4 10.6 * Labs Eliminated - 565, 1079 Autoclave Expansion (percent) 237-0.01 0.033 180 0.03 0.041 154 *225-0.01 0.018 107 0.02 0.018 75 * Labs Eliminated - 24, 32, 431, 493, 502, 515, 698, 2477, 2484, 4093, 4137, 4200 Summary of Results page 1 of 3

CCRL PROFICIENCY SAMPLE PROGRAM Portland Cement Proficiency Samples No. 203 and No. 204 Final Report Physical Results March 15, 2017 SUMMARY OF RESULTS Sample No.203 Test (unit) #Labs Average S.D. C.V. Average S.D. C.V. Air Content % (percent) 236 8.3 1.3 15 9.3 1.3 14 *232 8.4 1.1 13 9.3 1.1 12 * Labs Eliminated - 3297, 3801, 4051, 4200 Air Content - % Water (percent) 230 68.7 9.4 13.7 67.7 9.3 13.8 *216 69.9 2.3 3.3 68.9 2.5 3.7 * Labs Eliminated - 51, 60, 66, 101, 129, 692, 694, 1644, 3662, 3801, 4039, 4093, 4200, 4206 Air Content - Flow (percent) 232 86 3.5 4.1 89 3.4 3.8 No Labs Eliminated for This Test Compressive Strength - 3 day (psi) 259 3527 257 7.3 3687 241 6.5 *253 3537 232 6.5 3699 220 6.0 * Labs Eliminated - 39, 42, 360, 474, 1222, 3801 Compressive Strength - 7 day (psi) 259 4378 286 6.5 4357 270 6.2 *255 4385 265 6.0 4364 255 5.9 * Labs Eliminated - 9, 474, 1222, 3801 Compressive Strength - 28 day (psi) 244 5835 413 7.1 5381 364 6.8 *241 5846 390 6.7 5383 349 6.5 * Labs Eliminated - 360, 515, 958 Compressive Strengh - Flow (percent) 226 107 10 9.1 113 10 8.9 *222 108 9 8.1 114 9 8.1 * Labs Eliminated - 840, 2481, 3801, 4206 Summary of Results page 2 of 3

CCRL PROFICIENCY SAMPLE PROGRAM Portland Cement Proficiency Samples No. 203 and No. 204 Final Report Physical Results March 15, 2017 SUMMARY OF RESULTS Sample No.203 Test (unit) #Labs Average S.D. C.V. Average S.D. C.V. Fineness - Air Permeability (m²/kg) 250 395 17 4.2 450 18 4.1 *239 396 10 2.6 450 13 3.0 * Labs Eliminated - 4, 7, 24, 51, 52, 116, 252, 3606, 3819, 4200, 4206 Fineness - 45µm Sieve (percent) 233 95.12 4.04 4.25 97.06 0.46 0.48 *224 95.39 0.67 0.70 97.09 0.39 0.40 * Labs Eliminated - 18, 39, 132, 143, 219, 768, 2254, 2293, 3057 C1038 Mortar Bar Expansion (percent) 165 0.004 0.006 162 0.006 0.008 126 *155 0.003 0.003 97 0.005 0.004 68 * Labs Eliminated - 14, 26, 116, 121, 176, 203, 222, 1435, 4115, 4206 Summary of Results page 3 of 3

Normal Consistency - % Water 28.0 27.5 Normal Consistency - % Water (percent) 27.0 26.5 26.0 25.5 25.0 25.0 25.5 26.0 26.5 27.0 27.5 28.0 Normal Consistency - % Water (percent) Test No. 110 Normal Consistency - % Water 247 Points Ave 26.4 S.D. 0.45 C.V. 1.70 Ave 26.7 S.D. 0.46 C.V. 1.70 Labs Eliminated: 497, 557, 2477, 3850, 4080, 4137, 4200 Labs off Diagram: 25, 640

Vicat Time of Set - Initial 170 160 Vicat Time of Set - Initial (minutes) 150 140 130 120 110 100 90 100 110 120 130 140 150 160 Vicat Time of Set - Initial (minutes) Test No. 120 Vicat Time of Set - Initial 247 Points Ave 126 S.D. 12 C.V. 9 Ave 138 S.D. 12 C.V. 8 Labs Eliminated: 1715, 2462, 2477, 4142, 4206

Vicat Time of Set - Final 310 290 Vicat Time of Set - Final (minutes) 270 250 230 210 190 170 150 130 150 170 190 210 230 250 270 290 Vicat Time of Set - Final (minutes) Test No. 121 Vicat Time of Set - Final 236 Points Ave 219 S.D. 27 C.V. 12 Ave 240 S.D. 28 C.V. 12 Labs Eliminated: 8, 74, 132, 165, 1466, 3801, 4206 Labs off Diagram: 34

Gillmore Time of Set - Initial 240 230 220 210 200 Gillmore Time of Set - Initial (minutes) 190 180 170 160 150 140 130 120 110 100 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 Gillmore Time of Set - Initial (minutes) Test No. 130 Gillmore Time of Set - Initial 141 Points Ave 160 S.D. 22 C.V. 14 Ave 173 S.D. 20 C.V. 11 Labs Eliminated: 18, 408, 493

Gillmore Time of Set - Final 380 360 340 320 Gillmore Time of Set - Final (minutes) 300 280 260 240 220 200 180 160 140 160 180 200 220 240 260 280 300 320 340 360 Gillmore Time of Set - Final (minutes) Test No. 140 Gillmore Time of Set - Final 143 Points Ave 254 S.D. 36 C.V. 14 Ave 275 S.D. 33 C.V. 12 Labs Eliminated: 18

False Set - Paste Method 110 100 False Set - Paste Method (percent) 90 80 70 60 50 50 60 70 80 90 100 110 False Set - Paste Method (percent) Test No. 150 False Set - Paste Method 189 Points Ave 81 S.D. 8.0 C.V. 9.9 Ave 79 S.D. 8.4 C.V. 10.6 Labs Eliminated: 565, 1079

Autoclave Expansion 0.08 0.06 Autoclave Expansion (percent) 0.04 0.02 0.00 0-0.02-0.04-0.08-0.06-0.04-0.02 0.00 0 0.02 0.04 Autoclave Expansion (percent) Test No. 160 Autoclave Expansion 225 Points Ave -0.01 S.D. 0.018 C.V. 107 Ave 0.02 S.D. 0.018 C.V. 75 Labs Eliminated: 24, 32, 431, 493, 502, 515, 698, 2477, 2484, 4093, 4137, 4200

Air Content % 13.0 12.0 Air Content % (percent) 11.0 10.0 9.0 9 8.0 8 7.0 7 6.0 6 5.0 5 4.0 4 5.0 5 6.0 6 7.0 7 8.0 8 9.0 9 10.0 11.0 12.0 Air Content % (percent) Test No. 170 Air Content % 232 Points Ave 8.4 S.D. 1.1 C.V. 13 Ave 9.3 S.D. 1.1 C.V. 12 Labs Eliminated: 3297, 3801, 4051, 4200

Air Content - % Water 75.0 73.0 Air Content - % Water (percent) 71.0 69.0 67.0 65.0 63.0 61.0 62.0 64.0 66.0 68.0 70.0 72.0 74.0 76.0 Air Content - % Water (percent) Test No. 180 Air Content - % Water 215 Points Ave 69.9 S.D. 2.3 C.V. 3.3 Ave 68.9 S.D. 2.5 C.V. 3.7 Labs Eliminated: 51, 60, 66, 101, 129, 692, 694, 1644, 3662, 3801, 4039, 4093, 4200, 4206 Labs off Diagram: 2296

Air Content - Flow 94 92 Air Content - Flow (percent) 90 88 86 84 82 80 80 82 84 86 88 90 92 94 Air Content - Flow (percent) Test No. 190 Air Content - Flow 232 Points Ave 86 S.D. 3.5 C.V. 4.1 Ave 89 S.D. 3.4 C.V. 3.8

Compressive Strength - 3 day 4400 4200 Compressive Strength - 3 day (psi) 4000 3800 3600 3400 3200 3000 2800 3000 3200 3400 3600 3800 4000 4200 Compressive Strength - 3 day (psi) Test No. 200 Compressive Strength - 3 day 251 Points Ave 3537 S.D. 232 C.V. 6.5 Ave 3699 S.D. 220 C.V. 6.0 Labs Eliminated: 39, 42, 360, 474, 1222, 3801 Labs off Diagram: 9, 49

Compressive Strength - 7 day 5100 4900 Compressive Strength - 7 day (psi) 4700 4500 4300 4100 3900 3700 3500 3500 3700 3900 4100 4300 4500 4700 4900 5100 Compressive Strength - 7 day (psi) Test No. 210 Compressive Strength - 7 day 255 Points Ave 4385 S.D. 265 C.V. 6.0 Ave 4364 S.D. 255 C.V. 5.9 Labs Eliminated: 9, 474, 1222, 3801

Compressive Strength - 28 day 6600 6300 6000 Compressive Strength - 28 day (psi) 5700 5400 5100 4800 4500 4200 4600 4900 5200 5500 5800 6100 6400 6700 7000 Compressive Strength - 28 day (psi) Test No. 211 Compressive Strength - 28 day 241 Points Ave 5846 S.D. 390 C.V. 6.7 Ave 5383 S.D. 349 C.V. 6.5 Labs Eliminated: 360, 515, 958

Compressive Strengh - Flow 140 135 130 125 Compressive Strengh - Flow (percent) 120 115 110 105 100 95 90 85 80 80 85 90 95 100 105 110 115 120 125 130 135 140 Compressive Strengh - Flow (percent) Test No. 230 Compressive Strengh - Flow 222 Points Ave 108 S.D. 9 C.V. 8.1 Ave 114 S.D. 9 C.V. 8.1 Labs Eliminated: 840, 2481, 3801, 4206

Fineness - Air Permeability 490 480 Fineness - Air Permeability (m²/kg) 470 460 450 440 430 420 410 350 360 370 380 390 400 410 420 430 Fineness - Air Permeability (m²/kg) Test No. 270 Fineness - Air Permeability 237 Points Ave 396 S.D. 10 C.V. 2.6 Ave 450 S.D. 13 C.V. 3.0 Labs Eliminated: 4, 7, 24, 51, 52, 116, 252, 3606, 3819, 4200, 4206 Labs off Diagram: 146, 4150

Fineness - 45µm Sieve 99.00 98.50 Fineness - 45µm Sieve (percent) 98.00 97.50 97.00 96.50 96.00 95.50 95.00 93.00 93.50 94.00 94.50 95.00 95.50 96.00 96.50 97.00 Fineness - 45µm Sieve (percent) Test No. 281 Fineness - 45µm Sieve 223 Points Ave 95.39 S.D. 0.67 C.V. 0.70 Ave 97.09 S.D. 0.39 C.V. 0.40 Labs Eliminated: 18, 39, 132, 143, 219, 768, 2254, 2293, 3057 Labs off Diagram: 3607

C1038 Mortar Bar Expansion 0.015 0.010 C1038 Mortar Bar Expansion (percent) 0.005 0.0000-0.005-0.010-0.010-0.005 0.0000 0.005 0.010 0.015 C1038 Mortar Bar Expansion (percent) Test No. 400 C1038 Mortar Bar Expansion 155 Points Ave 0.003 S.D. 0.003 C.V. 97 Ave 0.005 S.D. 0.004 C.V. 68 Labs Eliminated: 14, 26, 116, 121, 176, 203, 222, 1435, 4115, 4206

CCRL PROFICIENCY SAMPLE PROGRAM Portland Cement Proficiency Samples No. 203 and No. 204 Final Report Heat of Hydration Results March 15, 2017 SUMMARY OF RESULTS Sample No.203 Test (unit) #Labs Average S.D. C.V. Average S.D. C.V. C186 Heat of Solution - Dry (cal/g) 27 577.0 13.3 2.3 581.0 31.0 5.3 *25 579.0 9.4 1.6 589.0 9.8 1.7 * Labs Eliminated - 2254, 4135 C186 Heat of Solution - 7 day (cal/g) 26 503.0 11.3 2.2 508.1 10.8 2.1 *25 504.5 8.5 1.7 509.5 8.3 1.6 * Labs Eliminated - 4135 C186 Heat of Solution 28 day (cal/g) 21 494.6 8.6 1.7 501.0 9.4 1.9 No Labs Eliminated for This Test C186 Heat of Hydration - 7 day (cal/g) 30 73.8 10.0 13.5 78.9 8.0 10.1 No Labs Eliminated for This Test C186 Heat of Hydration - 28 day (cal/g) 25 84.7 9.4 11.2 89.2 9.0 10.1 *24 85.9 7.3 8.5 89.9 8.5 9.5 * Labs Eliminated - 3057 C1702 Heat of Hydration - 3 day (J/g) 15 265 64 24.1 285 64 22.5 *13 285 12 4.2 310 12 3.9 * Labs Eliminated - 116, 3605 C1702 Heat of Hydration - 7 day (J/g) 14 300 76 25.4 318 76 23.9 *13 318 40 12.5 335 41 12.2 * Labs Eliminated - 3605 Summary of Results page 1 of 1

C186 Heat of Solution - Dry 610.0 C186 Heat of Solution - Dry (cal/g) 600.0 590.0 580.0 570.0 560.0 550.0 560.0 570.0 580.0 590.0 600.0 C186 Heat of Solution - Dry (cal/g) Test No. 291 C186 Heat of Solution - Dry 25 Points Ave 579.0 S.D. 9.4 C.V. 1.6 Ave 589.0 S.D. 9.8 C.V. 1.7 Labs Eliminated: 2254, 4135

C186 Heat of Solution - 7 day 530.0 525.0 520.0 C186 Heat of Solution - 7 day (cal/g) 515.0 510.0 505.0 500.0 495.0 490.0 485.0 480.0 485.0 490.0 495.0 500.0 505.0 510.0 515.0 520.0 525.0 C186 Heat of Solution - 7 day (cal/g) Test No. 292 C186 Heat of Solution - 7 day 25 Points Ave 504.5 S.D. 8.5 C.V. 1.7 Ave 509.5 S.D. 8.3 C.V. 1.6 Labs Eliminated: 4135

C186 Heat of Solution 28 day 520.0 515.0 510.0 C186 Heat of Solution 28 day (cal/g) 505.0 500.0 495.0 490.0 485.0 480.0 475.0 480.0 485.0 490.0 495.0 500.0 505.0 510.0 515.0 C186 Heat of Solution 28 day (cal/g) Test No. 301 C186 Heat of Solution 28 day 21 Points Ave 494.6 S.D. 8.6 C.V. 1.7 Ave 501.0 S.D. 9.4 C.V. 1.9

C186 Heat of Hydration - 7 day 110.0 105.0 100.0 95.0 C186 Heat of Hydration - 7 day (cal/g) 90.0 85.0 80.0 75.0 70.0 65.0 60.0 55.0 50.0 45.0 40.0 45.0 50.0 55.0 60.0 65.0 70.0 75.0 80.0 85.0 90.0 95.0 100.0 105.0 C186 Heat of Hydration - 7 day (cal/g) Test No. 290 C186 Heat of Hydration - 7 day 30 Points Ave 73.8 S.D. 10.0 C.V. 13.5 Ave 78.9 S.D. 8.0 C.V. 10.1

C186 Heat of Hydration - 28 day 115.0 110.0 105.0 100.0 C186 Heat of Hydration - 28 day (cal/g) 95.0 90.0 85.0 80.0 75.0 70.0 65.0 60.0 60.0 65.0 70.0 75.0 80.0 85.0 90.0 95.0 100.0 105.0 110.0 115.0 C186 Heat of Hydration - 28 day (cal/g) Test No. 300 C186 Heat of Hydration - 28 day 24 Points Ave 85.9 S.D. 7.3 C.V. 8.5 Ave 89.9 S.D. 8.5 C.V. 9.5 Labs Eliminated: 3057

C1702 Heat of Hydration - 3 day 335 325 C1702 Heat of Hydration - 3 day (J/g) 315 305 295 285 275 250 260 270 280 290 300 310 C1702 Heat of Hydration - 3 day (J/g) Test No. 500 C1702 Heat of Hydration - 3 day 13 Points Ave 285 S.D. 12 C.V. 4.2 Ave 310 S.D. 12 C.V. 3.9 Labs Eliminated: 116, 3605

C1702 Heat of Hydration - 7 day 450 430 410 390 C1702 Heat of Hydration - 7 day (J/g) 370 350 330 310 290 270 250 230 210 195 215 235 255 275 295 315 335 355 375 395 415 435 C1702 Heat of Hydration - 7 day (J/g) Test No. 510 C1702 Heat of Hydration - 7 day 13 Points Ave 318 S.D. 40 C.V. 12.5 Ave 335 S.D. 41 C.V. 12.2 Labs Eliminated: 3605