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Surprisingly, no significant loss in sensitivity or repeatability was observed for any of the elements stud- ied (Table 9). Furthermore, when a calibration that was prepared using oblong tablets was in turn used to test round tablets, no difference or bias was observed in the 30 March 2017 Tablets & Capsules Table 6 Repeatability Sample ID Cd (ppm) Pb (ppm) As (ppm) Hg (ppm) Co (ppm) V (ppm) Ni (ppm) Repeatability-1 0.91 1.06 3.03 5.33 10.65 21.26 40.73 Repeatability-2 1.08 1.16 2.98 6.05 10.59 20.62 40.90 Repeatability-3 1.15 1.17 2.95 5.53 10.12 20.19 40.41 Repeatability-4 1.02 1.17 2.94 5.47 10.28 20.25 40.22 Repeatability-5 0.97 1.11 2.93 5.22 9.98 20.94 40.72 Repeatability-6 0.97 1.04 2.98 5.74 10.06 21.03 40.55 Mean 1.02 1.12 2.97 5.56 10.28 20.72 40.59 Standard deviation 0.09 0.06 0.04 0.30 0.28 0.44 0.25 %RSD 8.52 5.17 1.23 5.40 2.74 2.10 0.61 Notes: Six individual samples were prepared at the 1J concentration containing the target elements. Acceptance criteria: %RSD ≤ 20% for each target element. Table 8 Specificity Sample ID Cd (ppm) Pb (ppm) As (ppm) Hg (ppm) Co (ppm) V (ppm) Ni (ppm) Hg pellet BLOD BLOD BLOD 112.09 BLOD BLOD BLOD Cd pellet 93.51 BLOD BLOD BLOD BLOD BLOD BLOD Pb pellet BLOD 103.09 BLOD BLOD BLOD BLOD BLOD As pellet BLOD BLOD 129.14 BLOD BLOD BLOD BLOD Co pellet BLOD BLOD BLOD BLOD 105.31 BLOD BLOD V pellet BLOD BLOD BLOD BLOD BLOD 104.82 BLOD Ni pellet BLOD BLOD BLOD BLOD BLOD BLOD 106.68 Notes: BLOD = below limit of detection. Each individual sample was spiked with only one ele- ment (at an approximate concentration of 100 ppm) and analyzed for all the target elements for interference. Acceptance criteria: The procedure must be able to unequivocally assess each target element in the presence of components that may be expected to be present, including other target ele- ments and matrix components. Table 7 Ruggedness Sample ID Cd (ppm) Pb (ppm) As (ppm) Hg (ppm) Co (ppm) V (ppm) Ni (ppm) Repeatability-1 0.91 1.06 3.03 5.33 10.65 21.26 40.73 Repeatability-2 1.08 1.16 2.98 6.05 10.59 20.26 40.90 Repeatability-3 1.15 1.17 2.95 5.53 10.12 20.19 40.41 Repeatability-4 1.02 1.17 2.94 5.47 10.28 20.25 40.22 Repeatability-5 0.97 1.11 2.93 5.22 9.98 20.94 40.72 Repeatability-6 0.97 1.04 2.98 5.74 10.06 21.03 40.55 Ruggedness-1 1.03 1.02 2.98 3.94 10.33 21.49 40.33 Ruggedness-2 1.05 0.99 2.94 4.68 10.45 19.63 40.78 Ruggedness-3 0.93 0.93 3.04 4.48 9.96 19.90 40.71 Ruggedness-4 0.86 0.94 2.99 4.38 10.09 19.51 40.56 Ruggedness-5 1.06 1.01 2.99 4.46 9.92 20.14 40.26 Ruggedness-6 1.05 0.81 3.06 4.76 9.98 19.58 39.80 Mean 1.01 1.03 2.98 5.00 10.20 20.38 40.50 Standard deviation 0.08 0.11 0.04 0.64 0.25 0.68 0.31 %RSD 8.07 10.59 1.40 12.84 2.49 3.34 0.76 Table 10 Precision: Repeatability (round tablet sets) Table 11 Comparison of random versus induced on-edge orientation of tablet sets Sample ID V (ppm) Co (ppm) Ni (ppm) Hg (ppm) Pb (ppm) As (ppm) Cd (ppm) Nominal 1J, 1 gram 100 50 200 30 5 15 5 Nominal 2J, 5 grams 40 20 80 12 2 6 2 Nominal 1J, 5 grams 20 10 40 6 1 3 1 Nominal 0.5J, 5 grams 10 5 20 3 0.5 1.5 0.5 Sample ID V (ppm) Co (ppm) Ni (ppm) Hg (ppm) Pb (ppm) As (ppm) Cd (ppm) Round 1J, 1 gram 96.8 (2.5) 50.0 (3.0) 197.8 (3.1) 33.3 (4.2) 5.0 (1.9) 15.1 (0.8) 5.4 (2.7) Round 2J, 5 grams 40.1 (2.7) 19.7 (2.8) 79.7 (1.4) 13.5 (2.9) 2.0 (6.1) 6.0 (2.5) 1.9 (8.3) Round 1J, 5 grams 20.5 (4.4) 9.5 (5.3) 40.4 (3.2) 5.4 (4.5) 1.0 (6.7) 3.1 (0.6) 1.1 (2.7) Round 0.5J, 5 grams 9.8 (4.9) 4.6 (3.8) 20.8 (1.5) 4.1 (3.6) 0.5 (40.7)* 1.6 (8.1) 0.4 (37.1)* Nominal concentrations for the target elements at the respective dosage Notes: Experimental repeatability data on round tablet sets analyzed against the calibra- tion curve for oblong tablet sets. Results are reported for triplicate analyses at each con- centration. Numbers in parentheses are %RSD. *The high %RSD represents the limit of quantification at the concentration containing the target elements under conditions analyzed. Sample ID V (ppm) Co (ppm) Ni (ppm) Hg (ppm) Pb (ppm) As (ppm) Cd (ppm) Random 40.1 19.7 79.7 13.5 2.0 6.0 1.9 On-edge 37.4 19.5 79.1 13.8 2.0 6.1 1.9 % deviation -6.7 -1.0 -0.8 2.2 0.0 1.7 0.0 Notes: Experimental repeatability data were gathered on round tablet sets that were randomly oriented and preferentially oriented. Average results are reported for triplicate analyses, and the % deviation of preferred orientation were compared to random orientation. Table 9 Precision: Repeatability (round tablets) Sample ID Cd (ppm) Pb (ppm) As (ppm) Co (ppm) V (ppm) Ni (ppm) Repeatability-1 1.07 1.26 3.15 10.85 21.01 42.88 Repeatability-2 1.01 1.55 3.09 10.52 21.77 42.88 Repeatability-3 1.08 1.11 2.98 10.57 21.23 42.02 Repeatability-4 0.98 1.10 3.13 10.61 21.69 43.85 Repeatability-5 0.94 1.24 3.13 9.57 20.88 41.81 Repeatability-6 1.07 1.04 2.92 10.73 22.33 42.53 Mean 1.03 1.22 3.07 10.48 21.49 42.66 Standard devisation 0.06 0.18 0.09 0.46 0.55 0.73 %RSD 5.61 15.14 3.08 4.38 2.54 1.71 Notes: Six individual samples (tablet sets) were prepared at the 1J (5-gram dose) concentration containing the target elements. Acceptance criteria: %RSD ≤ 20% for each target element.