Table 2.
Validation parameters of the total metal and metalloid analysis, recovery of CRMs using the ICP-MS technique
| Analyte | LOD [μg/L] | LOQ [μg/L] | U [%] | NCS DC 73309 | NCS DC 73310 | NCS DC 73312 | NIST 1643e | ||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| CRM [mg/kg] | Measured value [mg/kg] | R [%] | CRM [mg/kg] | Measured value [mg/kg] | R [%] | CRM [mg/kg] | Measured value [mg/kg] | R [%] | CRM [μg/L] | Measured value [mg/kg] | R [%] | ||||
| Mn | 0.03 | 0.1 | 10 | 2490 ± 84 | 2451 ± 249 | 98 | 1400 ± 47 | 1436 ± 144 | 103 | 240 ± 20 | 246 ± 25 | 102 | 38.97 ± 0.45 | 36.48 ± 3.6 | 94 |
| Co | 0.07 | 0.19 | 10 | 8.5 ± 0.8 | 8.19 ± 0.82 | 96 | 8.8 ± 0.7 | 8.31 ± 0.83 | 95 | 2.6 ± 0.7 | 2.04 ± 0.2 | 79 | 27.06 ± 0.32 | 26.15 ± 2.6 | 97 |
| Ni | 0.11 | 0.33 | 21 | 14.3 ± 1 | 14.78 ± 3 | 103 | 12.8 ± 1.3 | 12.49 ± 2.6 | 98 | 5.5 ± 1.4 | 4.59 ± 0.96 | 83 | 62.41 ± 0.69 | 59.051 ± 12 | 95 |
| Cu | 0.11 | 0.33 | 10 | 79 ± 3 | 79.4 ± 7.9 | 100 | 1230 ± 33 | 1231 ± 123 | 100 | 4.9 ± 0.5 | 4.29 ± 0.429 | 87 | 22.76 ± 0.31 | 20.039 ± 2 | 88 |
| Zn | 0.18 | 0.54 | 31 | 373 ± 14 | 310 ± 96 | 83 | 498 ± 18 | 430 ± 133 | 86 | 44 ± 5 | 13.5 ± 4.2 | 81 | 78.5 ± 2.2 | 48.54 ± 15 | 62 |
| As | 0.09 | 0.27 | 29 | 188 ± 13 | 190 ± 55 | 101 | 115 ± 6 | 115 ± 33 | 100 | 6.2 ± 0.6 | 5.4 ± 1.6 | 88 | 60.45 ± 0.72 | 52.85 ± 15 | 87 |
| Rb | 0.01 | 0.03 | 14 | 408 ± 11 | 540 ± 76 | 132 | 270 ± 10 | 350 ± 49 | 130 | 470 ± 23 | 379 ± 81 | 81 | 14.14 ± 0.18 | 15.58 ± 2.2 | 110 |
| Sr | 0.01 | 0.02 | 11 | 29 ± 4 | 23.4 ± 2.6 | 81 | 24 ± 3.0 | 20.9 ± 2.3 | 87 | ND | ND | ND | 323.1 ± 3.6 | 348.5 ± 38 | 108 |
| Ag | 0.01 | 0.03 | 10 | 3.2 ± 0.4 | 3.4 ± 0.34 | 108 | 1.15 ± 0.11 | 1.53 ± 0.15 | 133 | 0.066 ± 0.01 | 0.087 ± 0.01 | 132 | 1.062±0.07 | 1.027 ± 0.1 | 97 |
| Cd | 0.01 | 0.04 | 10 | 2.3 ± 0.2 | 1.8 ± 0.18 | 80 | 4.0 ± 0.3 | 4.13 ± 0.41 | 103 | 0.065 ± 0.01 | 0.063 ± 0.01 | 97 | 6.568 ± 0.07 | 5.94 ± 0.59 | 90 |
| Ba | 0.1 | 0.3 | 15 | 260 ± 17 | 175 ± 26 | 67 | 206 ± 15 | 160 ± 24 | 78 | 185 ± 24 | 87.0 ± 13 | 87 | 544.2 ± 5.8 | 504 ± 71 | 92 |
| Tl | 0.01 | 0.03 | 28 | 2.9 ± 0.4 | 3.41 ± 0.9 | 118 | 1.76 ± 0.27 | 1.63 ± 0.46 | 93 | 1.9 ± 0.4 | 1.88 ± 0.53 | 99 | 7.445 ± 0.1 | 7.91 ± 2.2 | 106 |
| Pb | 0.09 | 0.28 | 12 | 636 ± 22 | 659 ± 79 | 104 | 285 ± 11 | 296 ± 35.5 | 104 | 32 ± 5 | 31.8 ± 3.8 | 99 | 19.63 ± 0.21 | 20.23 ± 2.4 | 121 |
| Cr | 0.11 | 0.34 | 23 | 40 ± 3 | 35.5 ± 8.1 | 89 | 35 ± 3 | 25.6 ± 5.89 | 73 | 12 ± 3 | 8.11 ± 1.9 | 68 | 20.40 ± 0.24 | 21.33 ± 4.9 | 104 |
| Sb | 0.01 | 0.03 | 28 | 14.9 ± 1.2 | 15.0 ± 4.2 | 101 | 24 ± 3 | 25.4 ± 7.1 | 106 | 0.46 ± 0.12 | 0.66 ± 0.18 | 103 | 58.30 ± 0.61 | 56.83 ± 15 | 97 |
LOD limit of detection, LOQ limit of quantification, CRM the element content from the certificate of reference material, U uncertainty, R recovery, ND no data
Measured value-result of the elemental analysis of reference material after complete digestion using the ICP-MS technique