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GC-HS Variations Internal Standard Areas (Sample x Standard)

Posted: Tue Apr 19, 2005 2:11 pm
by Carlos Teixeira
Dear Friends,

Please, consider this situation:


We have been performing a new GC-HeadSpace (GC-HS) residual analysis with use of Internal Standard (IStd) and Reference Standard (RStd). The IStd and RStd areas have been almost equal (~2200ua and ~2750ua, respectivelly, with RSDs at ~2.5%). But the IStd areas in the sample injections have been reduced to 460ua with RSD at ~3.5%.
One important point must be considered because the Volatile Compounds Content of this sample is 80% and these volatile compounds have been limited the vials internal disponible space to presence of the IStd, wich probably present lowest Vapour Pressure over the HS conditions, so its areas for the sample must be lowest than the similar Reference Standard injections.

Normally, the IStd areas are equal to sample and Reference Standard injections, because the add quantity is the same for both.

Do you suggest different explanation for this?


Carlos Teixeira[/b]

sample preparation and spiking of stds

Posted: Tue Apr 19, 2005 8:16 pm
by chromatographer1
Carlos,

If you can explain your procedure (use different names if proprietary concerns are an issue) in preparing samples and stds I would be glad to discuss the issues you see. Or you may email me directly.

Rodney George
Senior Research and Development Scientist
Gas Separations Research
Supelco
595 North Harrison Road
Bellefonte, PA 16823

814-359-5737 voice
814-359-5459 fax
rgeorge@sial.com

Posted: Wed Apr 20, 2005 5:24 pm
by Mark
Carlos,
The other thing to consider is the effect of the drug on the internal standard recovery. Have you checked that you are getting a good recovery of the IS with the drug present?

Regards,
Mark