By JP Kucma on Wednesday, August 22, 2001 - 03:39 am:
I need to form a silyl ester from an acid and TMSCl. I can't remove excess of TMSCl du to the process. Is TMSCl a problem for the column (BPX5) or for the injector?
By Ron on Wednesday, August 22, 2001 - 05:38 am:
It is more often a problem for the detector. The TMSCl will tie up active sites in the injector and make it more inert, same with columns, but deposits in the detector may cause problems. There are often heavy, nonvolatile residues in samples that must be reacted with a derivatizing reagent, and these may have a negative effect on the inlet and column. It is a good idea to use a guard column for these samples, so you are cutting off the end of a cheap piece of tubing and not an expensive column.
By Jo Brodie on Wednesday, August 22, 2001 - 08:50 am:
Can you recover your silyl ethers in a solvent
in which your compound of interest is more
soluble than the excess reagent ?
By JP Kucma on Thursday, August 23, 2001 - 09:07 am:
Thank you for your help.
In fact, I do the silyl ester in dichloromethne, then I can remove TMSCl and CH2Cl2 by vacuum distillation and add toluene.
By shereen on Monday, June 14, 2004 - 02:04 am:
Iam working with urine sample on GC-MS using capillary column Igot a proplem with the column there is excess of TMSCl on it how I can remove it or wash it
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