“Old Wooden Bridge” Bridge to No Name Key from Big Pine Key, Florida Precision Statements for the Surface Resistivity of Water Cured Concrete Cylinders in the Laboratory by Mike Jackson for Mario Paredes Sponsors American Association of State Highway and Transportation Officials (AASHTO); Technology Implementation Group (TIG); Florida Department of Transportation; TRB Committee AFN30 – Durability of Concrete. Participants California Department of Transportation; Colorado Department of Transportation; Federal Highway Administration; Florida Department of Transportation; Florida Atlantic University; Grupo Carmelo, Puerto Rico; Indiana Department of Transportation; McGill University; Participants (Continued) Nebraska Department of Transportation; New York Department of Transportation; Puerto Rico Highways and Transportation Authority; Purdue University; Titan America –Tarmac; The University of North Florida; and Virginia Department of Transportation. Round-Robin Testing Program ASTM Designation C802, “Standard Practice for Conducting an Interlaboratory Test Program to Determine the Precision of Test Methods for Construction Materials.” AASHTO Designation: TP95-11, “Standard Method of Test for Surface Resistivity Indication of Concrete’s Ability to Resist Chloride Ion Penetration2.” Round-Robin Testing Program Fourteen (14) different laboratories; Twelve (12) different concrete mixtures; Wide range of constituent materials; and Two (2) different commercial SR meters: • CNS Farnell Ltd. • Proceq SA. Concrete Mix Constituents MICRON SILICA METATOTAL MICRON SILICA METAMIX CEMENT FLY ASH SLAG CA-1 CA-2 FA WATER FLY ASH SLAG FLY ASH FUME KAOLIN CEMENTITIOUS FLY ASH FUME KAOLIN NO. (LB/CY) (LB/CY) (LB/CY) (LB/CY) (LB/CY) (LB/CY) (LB/CY) (%) (%) (LB/CY) (LB/CY) (LB/CY) (LB/CY) (%) (%) (%) # 1 400 200 200 1785 1209 275 800 25.0 25.0 # 2 480 120 475 1439 1388 242 600 20.0 # 3 660 200 1323 1220 335 860 23.3 # 4 470 300 1585 1337 267 770 39.0 # 5 519 173 1532 1482 277 692 25.0 # 6 658 1800 1200 245 658 # 7 500 135 41 897 890 1157 270 676 20.0 6.0 # 8 423 141 935 2183 220 564 25.0 # 9 490 110 25 1740 1175 255 625 17.6 4.0 # 10 500 258 75 1700 1076 254 833 31.0 9.0 # 11 725 160 1741 972 265 885 18.1 # 12 677 75 1701 1052 263 752 10.0 w/cm FA/CA RATIO RATIO 0.34 0.40 0.39 0.35 0.40 0.37 0.40 0.39 0.41 0.30 0.30 0.35 0.68 0.73 0.92 0.84 0.97 0.67 0.65 0.70 0.68 0.63 0.56 0.62 Concrete Mix Constituents Mix w/cm ratios ranged from 0.30 - 0.41; Ten of the12 mixes contained fly ash; One mix contained no granular admixtures; One mix contained 25% slag; One mix contained 10% meta-kaolin; and Two mixes contained 4% - 6% silica fume. Test Samples Hardened 4-in. diameter by 8-in. long cylindrical concrete specimens were tested; Test specimens were fabricated by 12 of the participating labs, and shipped to all participants for SR testing; SR was measured in accordance with AASHTO Designation: TP95-11 after 28, 56, and 91 days of standard laboratory curing. Sample Packaging After 2 weeks of curing in lime saturated water, specimens were wrapped and sealed to avoid loss of moisture during shipping. Sample Shipping The specimens were then carefully packaged for 2nd Day shipping to avoid damage and/or drying during shipping. Surface Resistivity Testing SR was then measured after 28, 56, and 91 days of standard laboratory curing. Wenner Array Probe Resistivity Meter KOhm - cm Bottom Probe Spacing a =1.5" 8" 4" Top Example SR Test Results Surface Resistivity (SR) Readings (Kohm-cm) Sample # 0° 90° 180° 270° 0° 90° 180° 270° Average CTA-34 15.5 16 14.6 15.4 15.3 15.9 14.7 15.5 15.3625 CTA-36 15.3 16 14.7 15.2 15.3 15.6 14.6 15.1 15.2250 CTA-38 16.9 16.5 14.9 16.4 16.9 16.5 15.3 16.5 16.2375 Set Average 15.6083 Curing Condition Correction (x 1.1 lime tank or 1.0 for moist room) 1.1 Penetrability Based on Test 17.1692 Chloride Ion Penetration Type MODERATE Air Temperature of testing room (°F) 67 Water Temperature of lime bath (°F) 72 Curing history specific to your lab once you received the specimens Any abnormalities, comments, and/or notes. Mean SR at 28 Days LAB No. #1 #2 #3 #4 #5 #6 #7 #8 #9 # 10 # 11 # 12 # 13 # 14 MIX 1 11.254 11.250 11.238 11.858 12.367 10.509 14.792 11.500 11.188 10.800 0.000 10.683 0.000 0.000 MIX 2 9.088 9.046 9.026 10.208 15.854 9.447 12.792 9.000 9.763 9.604 9.733 8.875 10.042 9.933 MIX 3 8.996 8.729 8.275 10.358 10.421 9.165 12.458 9.667 9.133 9.475 11.063 9.517 10.785 9.663 Mean of 28-Day Surface Resistivity Readings (kOhm-cm) MIX 4 MIX 5 MIX 6 MIX 7 MIX 8 MIX 9 12.925 9.463 9.646 25.246 27.817 17.183 14.142 9.683 9.096 26.613 30.250 16.563 13.954 8.888 9.598 26.658 27.096 15.814 13.542 9.408 11.279 27.763 29.283 18.496 15.371 9.383 10.588 30.288 31.483 17.242 14.239 10.198 9.540 28.858 28.208 18.046 16.917 13.042 13.333 32.833 33.875 19.504 13.917 10.542 9.875 26.667 28.458 15.796 13.917 9.433 9.742 28.363 28.808 16.854 15.075 9.042 9.671 27.192 28.167 16.417 14.721 9.733 10.033 26.900 26.900 15.933 12.883 9.254 9.892 25.875 26.471 15.713 14.166 9.836 11.611 27.629 35.071 18.200 14.738 9.300 10.233 25.767 26.813 17.092 MIX 10 22.392 25.479 32.013 25.825 30.938 27.671 28.154 23.004 24.092 25.163 0.000 22.125 19.104 24.517 MIX 11 11.917 12.004 12.223 12.796 12.233 12.663 14.379 12.183 12.567 12.546 11.167 11.825 11.388 12.950 MIX 12 31.567 34.733 33.060 35.200 0.000 34.263 37.421 31.596 30.917 36.075 28.283 23.033 33.525 36.958 Note: Data shaded in yellow determined to be statistical stragglers by Mandel’s k-statistic. Std. Dev. at 28 Days LAB No. #1 #2 #3 #4 #5 #6 #7 #8 #9 # 10 # 11 # 12 # 13 # 14 MIX 1 0.49 0.37 0.43 0.38 0.45 0.13 0.29 0.25 0.15 0.17 0.00 0.69 0.00 0.00 MIX 2 0.39 0.24 0.31 0.20 0.72 0.58 0.36 0.66 0.14 0.54 0.38 0.12 0.22 0.23 Standard Deviation of 28-Day Surface Resistivity Readings (kOhm-cm) MIX 3 MIX 4 MIX 5 MIX 6 MIX 7 MIX 8 MIX 9 MIX 10 0.18 0.88 0.17 0.27 1.58 1.99 0.72 0.12 0.35 0.30 0.32 0.27 0.89 0.79 0.72 1.23 0.24 0.52 0.23 0.41 1.87 1.48 0.35 1.48 0.11 0.48 0.23 0.15 1.57 0.40 1.11 0.50 0.72 0.14 0.40 0.34 1.64 1.63 0.65 0.29 0.64 0.19 0.25 0.83 0.48 0.62 0.30 0.64 0.69 0.31 0.56 0.88 1.23 0.76 0.38 0.79 0.58 0.72 0.64 0.45 2.29 1.49 0.83 0.82 0.24 0.86 0.50 0.08 1.19 1.09 0.43 1.36 0.45 0.34 0.11 0.24 0.77 1.17 1.18 0.68 0.59 1.02 0.38 0.59 1.23 0.74 0.41 0.00 0.21 0.62 0.49 0.23 2.20 1.76 0.82 0.44 0.21 0.70 0.16 0.32 1.45 2.12 0.97 0.59 0.28 0.43 0.63 0.58 0.73 1.81 0.81 0.48 MIX 11 0.23 0.35 0.46 0.26 0.07 0.14 0.43 0.80 0.21 0.91 0.22 0.70 0.48 0.83 MIX 12 4.27 1.21 3.00 1.51 0.00 2.53 2.87 0.97 1.67 1.11 1.63 0.92 0.75 2.80 Note: Data shaded in yellow determined to be statistical stragglers by Mandel’s k-statistic. Mandel’s k-statistic at 28 Days 2.5 k = 2.044 at 1% significance MIX 1 2.0 MIX 2 k = 1.698 at 5% significance MIX 3 Mandel's k - Statistic MIX 4 MIX 5 1.5 MIX 6 MIX 7 MIX 8 1.0 MIX 9 MIX 10 MIX 11 MIX 12 0.5 Outliers Stragglers 0.0 #1 #2 #3 #4 #5 #6 #7 #8 Laboratory #9 # 10 # 11 # 12 # 13 # 14 Mandel’s k-statistic at 56 Days 3.5 3.0 MIX 1 MIX 2 Mandel's k - Statistic 2.5 MIX 3 MIX 4 k = 2.044 at 1% significance MIX 5 2.0 MIX 6 k = 1.698 at 5% significance MIX 7 1.5 MIX 8 MIX 9 MIX 10 1.0 MIX 11 MIX 12 Outliers 0.5 Stragglers 0.0 #1 #2 #3 #4 #5 #6 #7 #8 Laboratory #9 # 10 # 11 # 12 # 13 # 14 Mandel’s k-statistic at 91 Days 3.0 2.5 MIX 1 MIX 2 k = 2.044 at 1% significance MIX 3 Mandel's k - Statistic 2.0 MIX 4 k = 1.698 at 5% significance MIX 5 MIX 6 1.5 MIX 7 MIX 8 MIX 9 1.0 MIX 10 MIX 11 MIX 12 0.5 Outliers Stragglers 0.0 #1 #2 #3 #4 #5 #6 #7 #8 Laboratory #9 # 10 # 11 # 12 # 13 # 14 Mandel’s h-statistic at 28 Days 4.0 3.0 MIX 1 k = 2.298 at 1% significance MIX 2 2.0 MIX 3 Mandel's h - Statistic k = 1.850 at 5% significance MIX 4 MIX 5 1.0 MIX 6 MIX 7 0.0 MIX 8 MIX 9 MIX 10 -1.0 MIX 11 MIX 12 Outliers -2.0 Stragglers -3.0 #1 #2 #3 #4 #5 #6 #7 #8 Laboratory #9 # 10 # 11 # 12 # 13 # 14 Mandel’s h-statistic at 56 Days 4.0 3.0 MIX 1 k = 2.298 at 1% significance MIX 2 2.0 MIX 3 Mandel's h - Statistic k = 1.850 at 5% significance MIX 4 MIX 5 1.0 MIX 6 MIX 7 0.0 MIX 8 MIX 9 MIX 10 -1.0 MIX 11 MIX 12 Outliers -2.0 Stragglers -3.0 #1 #2 #3 #4 #5 #6 #7 #8 Laboratory #9 # 10 # 11 # 12 # 13 # 14 Mandel’s h-statistic at 91 Days 3.0 k = 2.298 at 1% significance 2.0 MIX 1 k = 1.850 at 5% significance MIX 2 MIX 3 Mandel's h - Statistic 1.0 MIX 4 MIX 5 MIX 6 0.0 MIX 7 MIX 8 MIX 9 -1.0 MIX 10 MIX 11 MIX 12 -2.0 Outliers Stragglers -3.0 #1 #2 #3 #4 #5 #6 #7 #8 Laboratory #9 # 10 # 11 # 12 # 13 # 14 Precision Calculations at 28 Days MIX 1 10 11.265 MIX 2 13 9.971 MIX 3 13 9.634 MIX 4 13 14.122 28-Day Surface Resistivity (kOhm-cm) MIX 5 MIX 6 MIX 7 MIX 8 MIX 9 13 13 13 13 13 9.551 10.062 27.217 28.833 16.873 0.151 0.169 0.174 0.375 0.149 0.174 2.187 2.015 0.256 3.265 0.617 0.428 0.155 0.450 1.169 0.407 3.434 0.790 0.803 0.304 0.624 sr 0.389 0.411 0.417 0.612 0.386 sR 0.638 1.853 0.889 0.896 COV (s r ) 3.45 4.13 4.33 COV (s R ) 5.66 18.59 s R /s r 1.64 r = 2.8s r R = 2.8s R Statistic P m sr 2 sL 2 sR 2 Outliers Lab # Type MIX 10 12 25.193 MIX 11 13 12.189 MIX 12 Pooled 12 Precision 32.434 Values 0.584 0.686 0.265 4.521 0.61 4.876 0.711 13.128 0.193 13.124 2.10 3.356 6.891 1.295 13.814 0.458 17.646 2.71 0.417 1.479 1.419 0.764 0.828 0.515 2.126 0.69 0.551 0.790 1.832 2.625 1.138 3.717 0.677 4.201 1.36 4.33 4.04 4.15 5.43 4.92 4.53 3.29 4.22 6.56 4.28 9.23 6.35 5.77 7.85 6.73 9.10 6.74 14.75 5.55 12.95 8.52 4.50 2.13 1.46 1.43 1.89 1.24 1.85 1.49 4.49 1.31 1.98 2.06 1.09 1.15 1.17 1.71 1.08 1.17 4.14 3.97 2.14 2.32 1.44 5.95 1.92 1.79 1 #7 h 5.19 1 #7 h 2.49 1 #7 h 2.51 1 #7 h 1.54 1 #7 h 2.21 1 #7 h 5.13 1 #7 h 7.35 1 #7 h 3.19 1 #7 h 10.41 1 #7 h 1.89 1 #7 h 11.76 1 #7 h 3.81 Note: Lab #7 Data Removed Based on Mandel’s h-statistic. Lab #7 Data Removed Precision Estimates at 28, 56, and 91 Days Lab Cured Age Variance (Kohm-cm)2 Standard Deviation (Kohm-cm) Precision (d2s) (Kohm-cm) Repeatable, (within lab) Reproducible (between lab) Repeatable (within lab) Reproducible (between lab) Repeatable (within lab) Reproducible (between lab) sr 2 sR 2 sr sR r R 28 0.61 2.71 0.69 1.36 1.92 3.81 56 1.63 12.9 1.09 2.97 3.05 8.33 91 3.64 33.1 1.55 4.24 4.34 11.9 (Days) Precision Statements Lab Cured Concrete Age COV (1s%) Precision (d2s%) Repeatability (within lab) Reproducibility (between lab) Repeatability (within lab) Reproducibility (between lab) (Days) COV (sr) (%) COV (sR) (%) r% R% 28 4.28 8.52 12.1 24.1 56 4.14 11.5 11.7 32.5 91 4.29 11.0 12.1 31.1 Proposed Precision Statements Single-Operator Precision – The results of two properly conducted tests by the same operator on concrete samples from the same batch and of the same diameter should not differ by more than 12.1% of their average. Multilaboratory Precision – The results of two properly conducted tests in different laboratories on the same material should not differ by more than 32.5% of their average. Bias - This procedure has no measurable bias. Equipment Equivalence Proceq SR Meter (kOhm-cm) 80 70 60 y = 1.02x - 4.12 R² = 0.97 Line of Equality 50 28 Days 40 y = 1.01x - 1.37 R² = 0.87 30 56 Days y = 0.99x - 1.83 R² = 0.97 91 Days 20 10 10 20 30 40 50 CNS SR Meter (kOhm-cm) 60 70 80 Paper Published in the Journal of ASTM International, Paper ID #JAI104268-11, “Precision Statements for the Surface Resistivity of Water Cured Concrete Cylinders in the Laboratory.”