Table 2.
An evaluation of M2+ interference-correction approaches on m/z 78 in reagent and regional tap water matrices fortified with Gd
| Reagent Water Fortified with Low and High Rare Earth Spikes | m/z 78, No Correction1,2 | m/z 78, No Correction1,3 | m/z 78, External Correction1,3,4 | m/z 78, In-Sample Correction5 | m/z 94, 8800 ICP-MS6 | High Resolution7 |
|---|---|---|---|---|---|---|
| 4.5mL He ([ppb] ± 2σ) | 2.5mL He ([ppb] ± 2σ) | 2.5mL He ([ppb] ± 2σ) | 2.5mL He ([ppb] ± 2σ) | 78→94 Se [O2] ([ppb] ± 2σ) | 78Se ([ppb] ± 2σ) | |
| 2 ppb Gd | 2.3 ± 0.7 | 0.7 ± 0.6 | −0.1 ± 0.6 | 0.0 ± 0.8 | 0.01 ± 0.04 | −0.03 ± 0.02 |
| 2 ppb Gd + spike8 | 3.1 ± 1.3 | 1.6 ± 0.9 | 0.8 ± 0.9 | 1.5 ± 1.3 | 1.0 ± 0.1 | 0.924 ± 0.004 |
| 50 ppb Gd | 53.0 ± 5.7 | 19.1 ± 1.9 | −1.0 ± 2.0 | −0.1 ± 1.2 | −0.04 ± 0.03 | −0.01 ± 0.12 |
| 50 ppb Gd+ spike8 | 54.0 ± 7.0 | 20.3 ± 1.8 | 0.0 ± 1.8 | 0.6 ± 2.3 | 1.1 ± 0.1 | 0.94 ± 0.06 |
| Regional tap waters9 | ||||||
| Water A + 50 ppb Gd, Nd, Sm | 51.2 ± 7.3 | 15.5 ± 2.9 | −9.6 ± 3.2 | −1.0 ± 2.6 | 0.18 ± 0.10 | 0.36 ± 0.03 |
| Water B + 50 ppb Gd, Nd, Sm | 51.1 ± 7.8 | 16.2 ± 2.0 | −9.3 ± 1.8 | −1.0 ± 3.9 | 1.35 ± 0.24 | 1.33 ± 0.12 |
| Water C + 50 ppb Gd, Nd, Sm | 51.8 ± 4.2 | 17.9 ± 4.3 | −7.3 ± 4.6 | 1.2 ± 4.2 | 2.29 ± 0.23 | 2.17 ± 0.26 |
| Water D + 50 ppb Gd, Nd, Sm | 53.3 ± 5.8 | 15.8 ± 2.5 | −9.6 ± 2.9 | −2.4 ± 3.5 | −0.03 ± 0.05 | 0.15 ± 0.02 |
| Water E + 50 ppb Gd, Nd, Sm | 53.2 ± 6.3 | 15.8 ± 3.6 | −10.3 ± 4.3 | −2.8 ± 4.2 | −0.01 ± 0.09 | 0.21 ± 0.01 |
| Water F + 50 ppb Gd, Nd, Sm | 52.5 ± 6.7 | 16.3 ± 3.8 | −9.6 ± 3.9 | −2.1 ± 1.9 | 0.33 ± 0.07 | 0.46 ± 0.05 |
Data were collected in normal resolution mode (0.8 amu at 10% peak height) using In as an internal standard with a 0.3-sec/amu integration time in selective ion monitoring mode. All estimates are based on 10 instrument replicates.
The calibration blank and 1 ppb standard associated with the analysis of reagent water (4.5 mL He) produced 9 cps and 67 cps, respectively. The calibration blank and 5 ppb standard associated with the analysis of regional waters (4.5 mL He) produced 12 cps and 169 cps, respectively.
The calibration blank and 1 ppb standard associated with the analysis of reagent waters (2.5 mL He) produced 23 cps and 87 cps, respectively. The calibration blank and 5 ppb standard associated with the analysis of regional waters (2.5 mL He) produced 31 cps and 279 cps, respectively.
The M2+ correction factors were estimated in narrow resolution mode (0.4 amu at 10% peak height) in an external rare earth standard and applied as a fixed correction factor to all samples. This correction also incorporated a narrow to normal conversion factor (see Figure 5).
Data were collected in narrow resolution mode (0.4 amu at 10% peak height) using In as an internal standard with a 0.3-sec/amu integration time in selective ion monitoring mode. All estimates are based on 10 instrument replicates. The M2+ correction factors were estimated in each sample. The solutions fortified with 2 ppb rare earth produced about 30 cps at the corresponding half-mass with %RSD across the 10 replicates of about 25%. The solutions fortified with 50 ppb rare earth produced about 300–500 cps at the corresponding half-mass with %RSD across the 10 replicates of 12%. A 1 ppb Se standard in narrow resolution mode using 2.5 mL He produces 51 cps with a 19 cps blank. All in-sample M2+ estimates required manual abundance-sensitivity evaluations at the adjacent masses to the M2+ ion.
Data were collected using m/z 94 in oxygen mode at 0.5 mL/min with a 0.99-sec/amu integration time in selective ion monitoring mode. All estimates are based on n = 5 using Y as an internal standard (YO+, 89→105). The calibration blank and 1 ppb Se standard produced 7 cps and 351 cps, respectively.
Selenium data were collected with an EScan over the mass range of 77.912–77.922 amu with a sampling time of 0.200 sec, 40 samples per peak, and 30% search and 60% integration windows over 3 runs and 2 passes (n = 6). All data were collected in high-resolution mode, and concentrations were determined relative to the 115In internal standard. The Auto Lock Mass feature was active during analysis.
This sample was fortified with 0.050 ppb As and 1 ppb Se.
All regional waters were prepared to reflect the 0.4% HCl concentration that results from an acid digestion according to Method 200.8.