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Author: Subject: Arkoma attempts 95% azeotropic EtOH
aga
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 Quote: Originally posted by arkoma *Y'all do get the pun, dontcha'?

A Star Redneck.

Er, yeah, ahem, we just didn't like to say er, anything, ahem.

I now got about 450ml near-azeo EtOH.

Also some tripot phos in the oven in a now-broken glass bowl

Was OK until i cranked the heat to 220 C.

macckone
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Use a copper reflux colum like everyone else. Three foot with intercooler will give nice reflux ratios 3 or 4 :1. The length and diameter are very dependent on heat input. You can get over 80% in a single run from mash and azeotropic on a second run after diluting to 50%. Discard the heads and tails. Primary contaminant is acetyal which gives a butter flavor. You can distill water out of vinegar a setup like this with 10:1 reflux ratios. But SS is better for corrossion resistance as acetic acid will corrode copper.
JJay
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I've used water-detecting paste that they sell at automotive stores to check for water in ethanol before (it's typically used for checking to see if you have coolant in your oil or water in your gasoline, etc.). Usually I just check the density (that's what ACS and USP suggest).

http://www.distill.com/specs/UK.html

I think you could add a small amount of anhydrous copper (II) chloride and look for a blue/green color to detect water, but I have not tried this... that might be a fun way to spend my Friday night.
Corrosive Joeseph
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My 300mm stainless tube column packed with a scrubber returned 91% EtOH in one run from my 'moonshine' starting material...........

Testing my 400mm tube soon. More to come....................

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arkoma
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I'm actually NOT drinking it. (Dumbass alert) and after checking my Vogel's (D'uh!!!)(facepalm) CaO, which I have.

 Quote: “Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.” and.. “The gentle reader will never, never know what a consummate ass he can become until he goes abroad.” Mark Twain, The Innocents Abroad

XeonTheMGPony
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*Edit: Clarified statement

Step one: Throw the radio out, it has no place in a lab! Especially when dealing with flammables

Step Two: Hit self very hard with solid object for even thinking of consuming a mind altering substance when working with flammables and setting foot into a lab *(Alcohol consumption + Lab = Darwin award)

Step three: Make a shield around the column but do not directly insulate

Step four: Ditch the oil do as others stated and used distilled water bath (We need very precise temp control here)

Step five: Start with low heat, allow every thing to saturate befor bringing the heat up, the slower you go the higher the purity you get!

All distillations are the same I find, precise temp control and taking your time, and ensuring a clean well lit lab with no distractions and a clear head = high purity results!

Only insulate your fractional column if you simply can not get the head temp to the target with slight increase in the heat source, but if this is required drop the heat source down, let the column balance then insulate a fraction, allow to balance and see where you end up befor increasing the heat source again.

If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up.

[Edited on 22-4-2016 by XeonTheMGPony]
arkoma
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 Quote: Originally posted by XeonTheMGPony If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up.

No. 250ml will last me a WHILE. I don't drink it. I've considered a 5 gallon still, only $200'ish, but nah. I'd get to thinking that I need to be SELLING the surplus. That would be all bad. *EDIT* And yes, my notes narrate a "comedy of errors". As in, "Don't do it this way". I'm 52 years old and live alone in a detached home. I also know I can screw up. I hope though that any younger/reckless/new to the hobby members read carefully and therefore don't have as cavalier an attitude. [Edited on 4-22-2016 by arkoma]  Quote: “Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.” and.. “The gentle reader will never, never know what a consummate ass he can become until he goes abroad.” Mark Twain, The Innocents Abroad aga Forum Drunkard Posts: 7030 Registered: 25-3-2014 Member Is Offline  Quote: Originally posted by arkoma CaO, which I have. Let us know how that works out. I tried it with oven-dried CaO and didn't get much drying of the EtOH at all. JJay International Hazard Posts: 3440 Registered: 15-10-2015 Member Is Offline Molecular sieves work great for removing the last of the water. They are a little pricey, but you can reuse them. XeonTheMGPony International Hazard Posts: 1594 Registered: 5-1-2016 Member Is Offline Mood: No Mood Quote: Originally posted by arkoma  Quote: Originally posted by XeonTheMGPony If you use ethanol allot it is well well worth building a dedicated unit out of copper, as it cuts down vastly on the time it takes in set up. No. 250ml will last me a WHILE. I don't drink it. I've considered a 5 gallon still, only$200'ish, but nah. I'd get to thinking that I need to be SELLING the surplus. That would be all bad.

I used to use huge volumes as a solvent and for fuel so I had a 56gallon feed still! and the reflux was made out of 3" diameter copper with a thermostatically controlled condenser lol.

and it came out at 90% in large volume. But for you doing small batch work I'd make 1L once you get it all set up right and store it some where cool and dry, to get it right in small scale is a royal pain in the rear, well worth making more then you need as you'll regret not doing so.

But the critical point is there is no rushing it, the slower you go with your temp, the finer the finished product, part of that temp control is having a good tight gradient on your column
arkoma
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 Quote: Originally posted by aga I tried it with oven-dried CaO and didn't get much drying of the EtOH at all.

I plan to take an Oxy-Acetylene torch to it to dry it. Heating to incandescence oughta do the trick. Vogel says DISTILL over CaO.

 Quote: “Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.” and.. “The gentle reader will never, never know what a consummate ass he can become until he goes abroad.” Mark Twain, The Innocents Abroad

aga
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Who is this Vogel dude ?

Bet it's PHDchemist in disguise

Just kidding.

If it's in Vogel's 3rd, it will probably work if done correctly !

(the 'correctly' part tends to trip me up a lot ...)

macckone
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You can't oven dry CaO. You need extremely high heat and low carbon dioxide.
zed
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Well, 95% I can buy at my corner liquor store. Not terribly expensive either.

But, Absolute is a very handy reagent, and harder to come by. Molecular sieves, you say? You have done this?

Lately?

macckone
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I will stick with my epsom salts and potassium carbonate. You need 3A molecular sieves.
aga
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 Quote: Originally posted by macckone You can't oven dry CaO. You need extremely high heat and low carbon dioxide

I put mine in an oven at ~ 220 C insead of the furnace.

This may easily explain why it didn't work.

[Edited on 25-4-2016 by aga]

Eddygp
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I would have added some dry (anhydrous) MgSO4 to the alcohol while distilling, as woelen suggested (CaSO4 is more of a hassle, MgSO4 can be easily removed!).
And yes, careful heating ensures efficiency; anti-bumping granules might be interesting if you really are having those problems - remember, safety is key, especially with hot flammable liquids!

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JJay
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I'm distilling some right now from 70% through a 30 cm Vigreux on a water bath. It's pretty slow going (approx 100 mL per hour) and might require another distillation to reach 95%.

Edit: From 950 mL of 70% v/v denatured ethanol, approximately 720 mL of distillate dripped over until nothing more came through the Vigreux. I haven't checked, but I already know that the concentration is pretty close to 95%; I could distill it a couple more times, but I'm just going to dehydrate it.

[Edited on 26-4-2016 by JJay]
arkoma
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oh, this is "pricy" alcohol for sure. Not the point.

 Quote: “Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.” and.. “The gentle reader will never, never know what a consummate ass he can become until he goes abroad.” Mark Twain, The Innocents Abroad

JJay
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Oh, right, if anyone wants to pay \$100/L for anhydrous ethanol, hit me up

[Edited on 26-4-2016 by JJay]
XeonTheMGPony
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 Quote: Originally posted by arkoma oh, this is "pricy" alcohol for sure. Not the point.

Pure near anhydrous Alcohol is very pricey! Lots of time, energy, material work goes into it on the lab scale.

That is why I do all my high investment synths in larger then needed batches, so when I need it all the work has all ready been don.
Velzee
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Where'd you get that pin, arkoma?

EDIT: Nevermind.

[Edited on 4/26/2016 by Velzee]

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Chemist_Cup_Noodles
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Hm, dehydrating your alcohols from what I've seen doesn't have to be too pricey. IIRC, you can use magnesium shavings and molecular seives. You might can get magnesium bits for free from a local machinist if you dig around hard enough. And molecular seives can be reusable if you dry them right. So this seems like a good way to go if you can wait a long time.

I found a pretty long JOC Article on drying your solvents that should be of good use: http://ccc.chem.pitt.edu/wipf/Web/Solvent_Drying.pdf

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arkoma
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@chemist_cup_noodles thanx for the paper KOH was never even on my radar.

 Quote: “Travel is fatal to prejudice, bigotry, and narrow-mindedness, and many of our people need it sorely on these accounts. Broad, wholesome, charitable views of men and things cannot be acquired by vegetating in one little corner of the earth all one’s lifetime.” and.. “The gentle reader will never, never know what a consummate ass he can become until he goes abroad.” Mark Twain, The Innocents Abroad

JJay
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I wonder how hard it would be to remove ketone denaturants with sodium bisulfite.

I probably shouldn't....
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 Sciencemadness Discussion Board » Fundamentals » Beginnings » Arkoma attempts 95% azeotropic EtOH Select A Forum Fundamentals   » Chemistry in General   » Organic Chemistry   » Reagents and Apparatus Acquisition   » Beginnings   » Responsible Practices   » Miscellaneous   » The Wiki Special topics   » Technochemistry   » Energetic Materials   » Biochemistry   » Radiochemistry   » Computational Models and Techniques   » Prepublication Non-chemistry   » Forum Matters   » Legal and Societal Issues