Posted: Thu Jan 15, 2009 11:07 am
Progress and responses
The phenol suite I'm looking at is phenol, mono and dimethyl phenols, nitrophenols, all the chlorophenols, nitrophenols and a couple of selected alkyl phenols.
Its a GC-MS method using a standard Agilent 6890/5973.
Derivitisation works well for the standards made from the same solvents used in the extraction so I am confident that they are moisure free. Unfortunately we don't have any KF equipment on site for any further tests.
Using additional derivitising agent worked, but required equal amounts of extract/BSTFA to work.
As things stand my manager has put a stop on further development for this project. He isn't happy using 1:1 of the derivitising agent so it looks like we will be going for using increased sample volumes and accepting the X10 dilution post elution as a necessary step and the increased LODs that will come from it.
I have one more idea left to try which is the aquasep cartridge from varian.
Sassman,
I like your idea of using diethylether and solvent changing. I'll probably come in this weekend and give that a shot.
As always, thank you all for your input. I'll post conclusions once the validation is complete.
Rich
The phenol suite I'm looking at is phenol, mono and dimethyl phenols, nitrophenols, all the chlorophenols, nitrophenols and a couple of selected alkyl phenols.
Its a GC-MS method using a standard Agilent 6890/5973.
Derivitisation works well for the standards made from the same solvents used in the extraction so I am confident that they are moisure free. Unfortunately we don't have any KF equipment on site for any further tests.
Using additional derivitising agent worked, but required equal amounts of extract/BSTFA to work.
As things stand my manager has put a stop on further development for this project. He isn't happy using 1:1 of the derivitising agent so it looks like we will be going for using increased sample volumes and accepting the X10 dilution post elution as a necessary step and the increased LODs that will come from it.
I have one more idea left to try which is the aquasep cartridge from varian.
Sassman,
I like your idea of using diethylether and solvent changing. I'll probably come in this weekend and give that a shot.
As always, thank you all for your input. I'll post conclusions once the validation is complete.
Rich