Page 49 - Application Notebook - PFAS Analysis
P. 49

No. SSI-LCMS-121




















                        Figure 3: Aggregate calibration curve for PFDA and example MRL 0.1 ng/L chromatogram.



















                       Figure 4: TIC of all 44 compounds at Level 7, 6 ng/L.

                                                                  All RSD results for the aggregate curve were less
                                                                  than 20%. All MRL level accuracies were between 50
                                                                  – 150%.  Accuracies at the MRL for each day
                                                                  (against the aggregate curve), and %RSDs are shown
                                                                  in Figure 6. Precision and accuracy studies in reagent
                                                                  water (RW) and tap water (TW) were  performed at
                                                                  10 ng/L and recoveries of majority of analytes were
                                                                  within 70-130% with %RSDs below 20% for all
                                                                  method analytes. The P & A study results were within

                                                                  EPA method  533 requirements; the data is included
               Figure 5: Blank: 80:20 MeOH: H2O.                  in Figure 7.

               ■ Results
               The use of a Phenomenex Gemini™ C18, 2.0 mm ID
               × 50 mm, 3.0 μm particle size  analytical column and
               a Shim-Pack XR-ODS 50 x 3.0 mm column as a delay
               column provided a good chromatographic separation
               for all compounds including branched and linear
               isomers. Calibration curves for PFAS analytes were
               prepared in the range of 0.025 – 25  ng/mL,
               representing pre-SPE sample concentrations of 0.1 –
               100 ng/L (except for NFDHA which was analyzed
               from 0.25 – 250 ng/L). All calibration curves
               (aggregate curve and 5 individual curves analyzed 15
               consecutive days) demonstrated r  values greater
                                          2
               than 0.99; the results are included in Table 2.
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