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Residual solvent analysis
Posted: Wed Nov 28, 2012 6:47 pm
by nitramyelood
Hi All
I am using a an Agilent HS G1888 to perform USP 467
i have real trouble running the CLAss 1 USP standard there are some dilutions as per the uSp and i find that by the time i run the sample the amount of RS present has reduced
Has anyone else seen this
Thanks
Nitram
Re: Residual solvent analysis
Posted: Wed Nov 28, 2012 9:43 pm
by chromatographer1
You are at the end of a very long line.
DO a search on this site about USP 467 and read about the problems many analysts are having with the method.
Welcome to the group.
Rod
Re: Residual solvent analysis
Posted: Sun Dec 02, 2012 3:17 pm
by krickos
Hi
As Rod stated there a bunch of known issues with the generic procedures, so please do a search.
The issue you seem to have is normally not related to dissolution steps, rather a sensitivity issue. (Ph Eur has a text where they recognize this issue at states that sample concentration (and consequently standards) may need increase).
Prepare the same concentration of class 1 solvents standards according both steps ie for waters soluble and non water soluble substances. Inject both and compare peaks and you will find something intresting.
/chris
Re: Residual solvent analysis
Posted: Wed Dec 05, 2012 8:14 pm
by RogerBardsley
There are 3 different temperautre settings for the headspace. Which one are you using.
I am an application chemist at Teledyne Tekmar and have not had an issue with Class 1 using the 80 deg C settings.