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Author: Subject: Distilliation by freezing
James Ikanov
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smile.gif posted on 5-8-2015 at 15:56
Distilliation by freezing


So I was doing some reading... and although aggravating, would it be possible to distill something such as H2O2 or HNO3 out of reliably water by freezing?

I have done a small batch (very tiny) of H2O2 and had some success reaching higher concentrations, but HNO3 seems like it might be more pesky.

I've tried making low concentrations using the Oswalt process, and I'm currently on version two of attempting to make a device that can reliably decompose Ammonium Nitrate into nitric oxides.

However, I usually end up with really low yields, unusably low.
I read that the freezing temperature of nitric acid is around -40 degrees...
would it be possible to distil low concentrations of nitric acid out to much higher ones by freezing the water it's mixed with?
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Steam
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[*] posted on 5-8-2015 at 16:37


HNO3 is a strong acid, meaning it will fully dissociate in water to form H+ and NO3 -. Similar to the way salt will dissolve in water. When it does this, the freezing point will be lowered. See "freezing point depression".

In short, no you can not, you would have to preform a standard distillation.




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BromicAcid
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[*] posted on 5-8-2015 at 18:06


Distillation involves actually converting a liquid to the gas phase then taking it back to a liquid. Freezing a liquid is quite different from a distillation. What you are suggesting is essentially a fractional crystallization, trying to crystallize a specific component of a mixture and leave the remainder liquid. Hydrogen peroxide as you have found out can be a good candidate for this method of purification, to a point. Issues that most people have involve mechanical losses and cooling too quickly resulting in occlusion and the whole mass turning into a useless chunk. Since most people are starting from 3% hydrogen peroxide it doesn't take much of a loss to cause a failed attempt. There are quite a few threads around here on the subject of concentrating hydrogen peroxide, some of those that touch more on freezing are:

http://www.sciencemadness.org/talk/viewthread.php?tid=1325
http://www.sciencemadness.org/talk/viewthread.php?tid=11382
http://www.sciencemadness.org/talk/viewthread.php?tid=30193

Just so you are aware the search engine around here is of limited utility, you are better off going to Google and searching for what you want with site:sciencemadness.org tacked onto the end of your search string.

I do disagree with Steam. I think that <u>in theory</u> nitric acid should be possible to freeze out, but the freezing point curve is a bumpy ride:

http://nitrogen.atomistry.com/physical_properties_nitric_aci...

From the chart theoretically you could might be able to get the HNO<sub>3</sub>*3H<sub>2</sub>O material to come out of your solution as the most concentrated since at temperatures below that that material would start to freeze out first. However, as with the H<sub>2</sub>O<sub>2</sub> issues caused by the high dillution, you may end up with the same problems, i.e., mechanical losses becoming significant. However, there are other ways to get nitric acid from ammonium nitrate without going through the trouble of decomposing to the nitric oxides but that's a subject for a different thread.




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