Residual solvent analysis

[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

[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

[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

[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.