Thomas Kelly wrote:
Joe,
    Thanks for the time you put into your response.
Re: Zeolites. I should probably buy some and experiment. I have a note to but 3A molecular sieve. I'll check to make sure that's the right one.
    As I understand it, with pressure constant, a liquid at boiling point does not increase in temp. as energy is added.
The energy (latent heat of vaporization) goes into producing the phase change. My impression was that the temp increase stalled at 150F even though I had the heater on.
Well then that's where the majority of methanol is coming off.  Remember that water vapour is also coming off at that temperature or even room temp for that matter.  I found that with vacuum if I opened the throttle I could make the reactor temperature drop even to the point that the heater coming on would not keep up with the energy loss due to the heat of vaporization. 
It rose very slowly to 160F, but at this point I turned the heater off and let the methanol flow. I gave it a bit of heat every now and then, but the temp stayed between 155 - 170F. This went on for hours and by then I had collected more than 4.5 gal (17.7L)  of methanol. It got late, I got tired and decided to just crank it up  ... leave the heater on. Above 160F the temp seemed to rise more quickly. Maybe much of the methanol had been removed  ---> less energy being used to evap methanol, more to heating remaining mix????
Yes as you recognized at some point here is an obvious increase in temp or decrease in vapour pressure which ever way you look at it. This is a logical endpoint or close to.  The question is really how much water can you live with.  Much of the literature says absolutely none but this is a relative thing. As you know there is always water and it's just a question of how much.  One day I should purposely do a set of tests with sequentially more water and find out.  If I had all the time and oil and chemicals in the world....
     I'm not through with this yet. In fact I have plenty more glycerine/methanol to try.
snip
 
Is this the idea?
    Knowing the conc. of radioactive water in the ethanol/water mix, the amount of radioactive water remaining in the ethanol after treating w. the zeolite would allow calc. of the amount of water removed.
Exactly.  The amount of radioactivity in the solvent after drying is a direct indication of the amount of heavy water.  Hard to measure such small amounts otherwise! We are talking about PPB or ones'ys and twos'ys of PPM.


Joe
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