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I have 50 ml of a compound I would like to purify. Since the impurities presents have close boiling points (b.p.), I have to use fractional distillation. Am I going to lose significant quantity of my product volume because of loss related to the distillation itself?

If so, what can I do to minimize the loss?

I thought about adding a higher b.p. solvent to the distillation flask so I can distill all the compound without leaving some in the flask. What do think about this method?

Are there any other strategies?

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    $\begingroup$ Adding a chaser is certainly necessary to maximize yield. $\endgroup$ – Lighthart Feb 12 '16 at 22:54
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In order to both achieve sufficient separation and minimize loss during fractional distillation, you want

  • a large inner column surface for optimal contact of the vapour phase (upstream) and the liquid phase (downstream)
  • a rather small inner column volume

Often, these destillation are performed using a Spaltrohr distillation apparatus. Here, the vertical column consists of two concentrical, threaded glas tubes with a gap of 1-2 mm in between.

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