Re: Gravimetric Analysis.

rain.on.moon@xxxxxxxxx wrote:
>
> Dear All,
> I am in the middle of nowhere. I have had a reaction to synthesize
> tributyl phosphate.

You buy it, $28/liter.

> The reactants were phosphorus oxychloride,pyridine
> and n-butanol. Now that the reaction is complete. I want to get the
> organic layer separated in the separating funnel analysed. I want to
> know how much quantities of tributyl phosphate, dibutyl phosphate,
> monobutyl phosphate, water and butanol are present in the separated
> organic layer.

Distill the POCl3 (aspirator vacuum) so it is clean. What precautions
must you take during and after the distillation? Excess *dry* butanol
(93 C azeotrope, 43% water) and do the reaction in ether so py.HCl
precipitates to make workup easier. Filter; wash the filter cake.
Rotovap.

TLC to monitor how things are going. Partially esterified phosphates
will have some detergent character. Good luck, buddy.

> I have searched for all th available methods of analysis
> but they are qualitative. I want to know if there is any method that
> gives us the percentage of the above mentioned entities. Any sort of
> help will be appreciated.

Now you're worried how things turned out? The time to worry is before
you do it. If you do it right you don't worry about
non-stoichiometric reaction channels - because you have been
pro-active in preventing them them. NMR, proton and P-31.

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

Relevant Pages

  • Gravimetric Analysis.
    ... Now that the reaction is complete. ... organic layer separated in the separating funnel analysed. ... know how much quantities of tributyl phosphate, dibutyl phosphate, ...
    (sci.chem)
  • Re: Gravimetric Analysis.
    ... Now that the reaction is complete. ... > organic layer separated in the separating funnel analysed. ... > know how much quantities of tributyl phosphate, dibutyl phosphate, ...
    (sci.chem)