Preparing for ICAL - vivianlu9/EMAX_VOA_sandbox GitHub Wiki
General Checklist
- Prepare new IS, SS, 1° and 2° standards.
- Bake out a brand new trap.
- Retune the instrument.
- Test new standards to make sure they're prepared correctly.
- Test the tune to make sure you can see LOD for all compounds AND that the tune check consistently passes. Adjust as needed.
Testing Standards
Prepare two tests, one with the 1° standards and the other with the 2° standards. Overlay the chromatograms or generate a Matrix Spike/Duplicate Recovery Report to compare the compound recoveries. They should be reasonably close (within ~10% is good).
We don't care about the actual recovery values since the instrument is being recalibrated anyway. We only care that the recoveries are close.
If one of the values looks drastically different, recalculate the tests using an ICAL where the ICV passed evaluation to determine which one is incorrect. Make sure you're using an ICAL where the 2° was used for the ICV (some ICALs...do not).
Testing the Tune
Prepare tests at LOD levels for the analysis being calibrated. You should be able to see all of the qualifier ions at LOD.
Usually these values will be 0.2ppb, 0.3ppb, and 0.5ppb for 8260 25mL and 524.2. For APP IX it's 0.5, 1.0, and 2.0ppb.
[insert pic of LOD here]
If you can't see the qualifier ion at the current settings, you may need to increase the EM. Alternatively, you may need to lower the threshold for the specific runtime, but we don't usually need to adjust those settings.