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Buffers and Degassing

Posted: Mon Jun 13, 2005 2:07 pm
by ravenwork
Greetings,

I are performing gradient RP HPLC for environmental analysis. I usually pump pure solvents with low pressure mixing, and He sparging.

I am seeing some unacceptable retention time shifts with a new method. The shifts appear to be sample matrix related. I suspect a pH effect since we are running unbuffered with pure solvents.

I would like to try buffering the water. Phosphate is not a good choice since the samples contain calcium chloride. I want to try a formate buffer, but I am concerned about its volatility. Since we generally use pure solvents, we just sparge continuously. Am I right in thinking that continuous sparging of a formate buffer may change its pH over time due to evaporation of the formic acid? Can I sparge for 30 minutes and then maintain a He blanket in the vessel?

ravenwork

Posted: Mon Jun 13, 2005 3:17 pm
by tom jupille
Probably 5 minutes of sparging will suffice.

Posted: Mon Jun 13, 2005 7:03 pm
by Kostas Petritis
I used in the past a similar mobile phase with a Dionex (LC-Packings) nano-pump and I didn't observe any problems of formic acid evaporation. Once you prepare the mobile phase you start by sparging relatively intensively, then after 5 minutes you decrease the He flow rate to a minimum...