Re: Drying of Alcohols.

rain.on.moon@xxxxxxxxx wrote:
>
> Dears,
> I am involved in my MS thesis nowadays. The problem I am having at the
> momenet is that I have 1-Butanol (n-Butanol)which has a minimum
> concentration of 99%. Rest are some impurities with water. I want to
> remove all the traces of water from this alcohol. Apart from Molecular
> Sieves and Distillation, what is the most suitable process to
> accomplish the task of drying 1-Butanol? Please let me know the
> details. Waiting anxiously your responses.

Running down a column of freshly activated 3A molecular sieves won't
dry it? How 'bout a column of Woelm Activity 0 alumina after the
sieves? Distill under dry inert gas from Na butoxide or Mg butoxide
(Mg turnings, a teensy of iodine, reflux until the metal dissolves,
distill).. but that gives you added organic impurities.

What does "remove all the traces of water" mean? 100 ppm H20? 1 ppm
H2O? 1 ppb H2O? Dry by Karl Fisher titration (Hydranal, please)?
All your glassware flamed under vacuum? Opening the pot to air will
give you at least 10 ppm water contamination instantly. So will
glassware "dried" at 110 C.

How dry is your glovebox? Does Me3Al fume white when opened? (Me3Al
evaporates like water - don't pour it intoa dish. In fact, don't even
think about Me3Al until you see the safety video.) Does a freshly cut
Na surface tarnish?

--
Uncle Al
http://www.mazepath.com/uncleal/
(Toxic URL! Unsafe for children and most mammals)
http://www.mazepath.com/uncleal/qz.pdf
.

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