Test parameter | Acceptance criteria | Results for EMS |
---|---|---|
System suitability | %RSD for peak area response (n = 6) | Day-1: 1.6% Day-2: 0.69% |
Specificity | Interference from blank | No interference |
Sensitivity | Concentration | LOD—0.62 ppm LOQ—1.02 ppm |
S/N for LOD solution should be > 3:1 | 4:1 | |
S/N for LOQ solution should be > 10:1 | 15:1 | |
RSD for six replicate LOQ solution injections should be ≤ 15.0% | 2.58 | |
Linearity | Range | 1.02–50 ppm |
Calibration Equation | y = 297x + 770.9 | |
r2 | 0.9997 | |
Residual plots | Random scatter | |
Precision | Average recovery (n = 6) from the spiked samples performed at 100% level; RSD should be ≤ 10.0% | 93.6%; 5.4% |
Accuracy | Average recovery (n = 3) from the spiked samples performed at 5 levels—LOQ—200%; RSD should be ≤ 10.0% | LOQ—90.3%; 7.2% 50%–90.9%; 6.5% 100%–95.8%; 1.5% 150%–105.3%; 1.9% 200%–102.6%; 1.1% |
Intermediate precision (Analyst 2) | Average recovery (n = 6) from the spiked samples performed at 100% level; RSD should be ≤ 10.0% | 96.9%; 3.6% |
Solution stability | Standard and 100% spiked solution stored at ambient laboratory conditions (25 ± 5 °C) and refrigerated conditions (2–8 °C) were studied for 48 h | Stable for 48 h |
Robustness | RSD (%) for peak area response (n = 6) with 0.8 flow rate %Recovery (n = 3) for 100% spiked solution with 0.8 flow rate | 2.4% 95.6% |
RSD (%) for peak area response (n = 6) with 1.2 flow rate %Recovery (n = 3) for 100% spiked solution with 1.2 flow rate | 1.8% 91.4% | |
RSD (%) for peak area response (n = 6) with 1.3 mL/min gas flow %Recovery (n = 3) for 100% spiked solution | 5.3% 102.8% | |
RSD (%) for peak area response (n = 6) with 1.8 mL/min gas flow %Recovery (n = 3) for 100% spiked solution | 2.2% 93.5% |