Flash column chromatography equilibration speed – how fast can you go?

Equilibrating silica flash chromatography columns is something I always do.  There are chemists who see this as an unnecessary, time-and-solvent-wasting step.  Because getting consistent, predictable results is a priority, I equilibrate to remove the variability that can be caused by heat generated as solvent initially contacts the silica. Consistency is really important when running flash column chromatography because re-runs are time consuming and may put your compound at risk.

In this post, I examine the role of equilibration speed and duration to show its impact, or lack there of, on purification performance.

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Published by

Bob Bickler

Technical Specialist, Biotage

2 thoughts on “Flash column chromatography equilibration speed – how fast can you go?”

  1. Hello Bob

    I always equilibrate my columns and do it manually. I think I have mentioned before that I start off with the most polar solvent and pump at full speed until the heat has dissipated then hit the button to equilibrate to the starting conditions for at least 1CV. I was told a long time ago that this speeds up the equilibration. If I am using dichloromethane/ MeOH then I would equilibrate for 3CV at the start point which would be 1% MeOH.
    I’ve never seen a column melt though! It seems reasonable that a relatively long column would result in more heat by the time the hot band leaves the column. Our longest columns are also the heaviest and when I’ve used 3Kg columns I know that when the hot band leaves these columns there is no liquid, only very hot vapour. Flow rate is 900ml/min and it’s a bit scary, just hope everything is well earthed or you could have a flame thrower.
    Will the Sfär columns be available as reverse phase in the near future?

    1. Hi Derek,

      Thank you for sharing your experiences, I find your equilibration technique intriguing. Equilibrating in the polar solvent is not something I do but if it works for you then stay with it. To speed equilibration we have actually moved to a shorter duration (2CV) but at very fast flow rates (150 mL/min with 5 and 10 gram columns) with the starting gradient blend. We find this works very well and columns are equilibrated in seconds.

      Reversed-phase Sfar columns are available though they have standard surface area but do have a 25-30 um particle diameter.

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