552

Discussions about sample preparation: extraction, cleanup, derivatization, etc.

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552

Anyone out there using an internal standard that can be added to the MTBE extraction solvent? I really don't like the post extraction spiking of 1,2,3-TCP.
EPA 552.3 uses the ISTD in the extraction solvent, we have found it works quite well. I have less extraction variablity and better recovery, probably due to using more acid at derivatization and no CuSO4. I also use a different surrogate, the method surrogate has given me wildly different results between batches/technicians.
Have any of you had any problems with interferences in the chromatograms when doing 552.3? I'm seeing a large number of interference peaks all over my chromatogram especially near the surrogate on my primary column I have very consistent recoveries on one column whereas on the column the results seem to be all over the place.
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