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Author: Subject: Arkoma attempts 95% azeotropic EtOH
Chemist_Cup_Noodles
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[*] posted on 26-4-2016 at 10:21


Quote: Originally posted by JJay  
I wonder how hard it would be to remove ketone denaturants with sodium bisulfite.

I probably shouldn't....


If you think you'd feel inclined to test the fruits of your labor personally, maybe you shouldn't. But I'd still it for science (heh). I think it would be a neat experiment to carry out, and quite a fun and interesting process. Kinda like a puzzle. Because in theory denaturants are meant to make the alcohol unfit for consumption, even after distillation or chemical means, but that is certainly untrue. Where there is a will there is a way. So go for it.




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JJay
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[*] posted on 26-4-2016 at 20:47


I don't think that's a good idea, really... for one thing, it would be likely to leave some sulfur dioxide in the ethanol after distillation (which would require further distillation from, for example, sodium carbonate).

For another, removing denaturants is almost certainly illegal.
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XeonTheMGPony
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[*] posted on 27-4-2016 at 04:45


Quote: Originally posted by JJay  
I don't think that's a good idea, really... for one thing, it would be likely to leave some sulfur dioxide in the ethanol after distillation (which would require further distillation from, for example, sodium carbonate).

For another, removing denaturants is almost certainly illegal.

So is some of the stuff you do in home chemistry and the entire energetics board in some countries

It is the intent that determines if it is illegal IMO, and that is how our legal system mostly works too (Canada) SO if he where doing it to sell then yes, but just purifying a reagent for usage at home no.

It wouldn't be worth the cost for any one of concern to hassle him.
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JJay
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[*] posted on 27-4-2016 at 05:11


Eh, I follow the law. Technically, when distilling denatured ethanol without a license, you have to be recovering it from some other process, which is why I wiped my *ss with it before distillation (I left out that part), but I'm in the clear here.
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Chemist_Cup_Noodles
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[*] posted on 27-4-2016 at 06:12


Quote: Originally posted by XeonTheMGPony  
Quote: Originally posted by JJay  
I don't think that's a good idea, really... for one thing, it would be likely to leave some sulfur dioxide in the ethanol after distillation (which would require further distillation from, for example, sodium carbonate).

For another, removing denaturants is almost certainly illegal.

So is some of the stuff you do in home chemistry and the entire energetics board in some countries

It is the intent that determines if it is illegal IMO, and that is how our legal system mostly works too (Canada) SO if he where doing it to sell then yes, but just purifying a reagent for usage at home no.

It wouldn't be worth the cost for any one of concern to hassle him.


Well but why would you get "busted" for doing this? As long as you're not buying gallons and gallons of denatured alcohol or trying to sell your de-denatured product, I don't see where any issues should arise. If you're worried about neighbors seeing you doing experiments and calling the police, I wouldn't be. I live in the suburbs and I've done some experiments in my back yard (I lack a fume hood and I don't want to burn my house down), and no one has ever said anything other than just being curious about my "lab equipment". So as long as it doesn't look like you're running a huge meth operation, I really wouldn't worry about following the law perfectly. But worst case scenario, for some random reason if the police found out that you removed denaturant from just a small amount of alcohol, they give you a ticket and a small fine for doing it without a license.




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[*] posted on 30-4-2016 at 09:32


I do stuff in the backyard. One house adjoining ours is unoccupied, one is a close friend of the family who couldn't be suspicious of me, and the other two *I'm* suspicious of, so I don't worry too much. I've also told friends of my lab, and had to deal with guidance counselors on the subject, so I'm slightly experienced in dealing with such...



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[*] posted on 8-5-2016 at 05:20


Last year I used to distill 92-95% EtOH with 2" stainless steel wool packed active reflux still so it is doable, but it could require extensive steps with small scale glassware. The odorous and tasteous properties of the product will improve significantly if it is to be processed with activated carbon and sodium carbonate at 50% dilution after first concentrative distillation and redistilled.

[Edited on 8-5-2016 by Refinery]
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Corrosive Joeseph
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[*] posted on 31-5-2016 at 22:36


Quote: Originally posted by Refinery  
Last year I used to distill 92-95% EtOH with 2" stainless steel wool packed active reflux still so it is doable, but it could require extensive steps with small scale glassware. The odorous and tasteous properties of the product will improve significantly if it is to be processed with activated carbon and sodium carbonate at 50% dilution after first concentrative distillation and redistilled.

[Edited on 8-5-2016 by Refinery]


Could you explain your process a little please................?




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Corrosive Joeseph
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[*] posted on 1-6-2016 at 23:18


Sorry for the double post, l can't edit....................

As l promosed l would report back with results so here goes....................

58% ran through the 300mm length 30mm dia stainless steel tube column stuffed with half a scrubber yielded 91%

58% ran through a 500mm length 32mm dia stainless steel tube column stuffed with a full scrubber yielded 91%

91% ran through the 500mm column once again yielded about 93.5%.....................


Comments and criticisms welcome please =)


CJ

[Edited on 2-6-2016 by Corrosive Joeseph]




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[*] posted on 2-6-2016 at 11:48


Wouldn't the fact that KOH is soluble in ethanol be a problem?
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[*] posted on 25-6-2016 at 13:43


UPDATE.

Having made a few slight procedural changes, I have reached 92% via distillation. I used about 10 feet of 10ga copper wire cut into short pieces and bent in curlicues. These I used to pack a claisen adapter. Hit an old dinner plate with a hammer and voila, boiling chips. Also swapped out the oil bath for a water bath.

The packed claisen works much better than my 300mm Vigreux. I see an "old school" fractionating column on my shopping list.........

I have approx 450ml of the 92%, and am planning to distill it over CaO. If I can beat the azeotrope by even one or two percentage points the whole Ark-La-Tex will hear my whoops of triumph.





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[*] posted on 25-6-2016 at 14:13


Using some kind of reflux column is much Smarter than not doing.

A stripping run, collecting everything up to around 88 C never hurts, followed by a temperature-specific run where you Only collect everything at 78~79 C, provided that the thermometer is calibrated.

That was todays' fun !

If it had to be gehtto'd and azeo++ on the second run, i'd use the Thumper idea and part-fill the thumper with oven dried tripotassium phosphate.

Since my first attempt at tri-pot-phos i have not been able to successfully make it again.

I am pretty sure the 'pure' KOH i bought from some dodgy geezer in a Turkish kasbah is actually KOH/KCl mixed, which seems to screw it up.

My original batch of KOH was from a much more reputable source, but got used up in the first tri-pot-phos experiments.

Some A3 molecular sieves arrived yesterday.

How to dry and test them for 'activity' ?

Well, stick them in the oven at 250 C for 3 hours and see what happens.

Result : They get hot.

After being allowed to cool for 10 minutes, they were warm, but easy to handle, so a couple of spatulas were held in the expendable left GLOVED hand and a squirt of water was put on them from the wash bottle (found that test embedded in some discourse on how to dry sieves).

They immediately got too hot to be safe, and were thrown with great speed into the void.

This apparently signifies that :-

a) these molecular sieves are indeed 'activated' by 3 hours at 250 C

b) i have less molecular sieves now




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[*] posted on 25-6-2016 at 14:30


92% was achieved on the third run.

My starting "substrate" this time around was wine made from Ar-Kin-Saw blackberries and Montrachet yeast. My Chinese thermometers ain't that accurate, so first run I kept everything up til about 90c. That yielded 50% EtOH. Second run I did by VOLUME, 500ml in the flask, discarded the first 30ml, and kept the next 200ml. There were a lot of "second runs", but not as many as it took to gather up an appreciable qty of 50% (I am limited as my biggest RBF is 1000ml). Second run was averaging about 80% EtOH. Slow careful fractionating through my packed claisen on the third run got me to 92%. My Chinese thermometer sat rock steady at 82c (like I said, not real accurate).


edit--spelling
Not "ghettoing". I can BUY 95% Everclear for WAYYYYY less time and money. But where is the fun in that?

[Edited on 6-25-2016 by arkoma]





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and..

“The gentle reader will never, never know what a consummate ass he can become until he goes abroad.”

Mark Twain, The Innocents Abroad

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aga
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[*] posted on 25-6-2016 at 14:47


Calibrate your thermometers maybe ?

Glass of water with lots of ice, thermometer should read 0 C.
Whatever the reading is, y1 = 0, x1 = the thermometer reading.

Boil some water, thermometer should read 100 C.
Whatever the reading is, y2 = 100, x2 = the thermometer reading.

Mathematically, if y is the actual temperature and x is what the thermometer says, then :
$$y = mx + c$$
If you do the algebra, it works out that
$$m = \frac {y2 - y1}{x2-x1}$$
In this case y2=100 and y1=0 so we can simplify it to :
$$m = \frac {100}{x2-x1}$$
$$c = 100 -mx_2$$
Once you know the 'm' and 'c' values for that particular thermometer, you can easily work out the accurate exact temperature based on what it reads by feeding the x (thermometer reading) back into the equation :
$$y = mx + c$$
... y being the actual exact temperature, no matter how 'wrong' the thermometer reading seems.

Any thermometer, especially a digital thermometer for a few bucks off ebay still needs calibrating in this way if you want it to be accurate.

[Edited on 25-6-2016 by aga]




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[*] posted on 25-6-2016 at 18:04


Don't forget to allow for altitude differences. 300 ft above sea level will make a big difference when compared to 7500ft.
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[*] posted on 25-6-2016 at 18:25


At 7500 the azeotrope has about 96% alcohol.
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[*] posted on 26-6-2016 at 18:59


Huh, so starting a lab at a certain, different than average altitude could let you produce better than standard azetrope...

Why waste such fine wine? What happened to using cane sugar and tomato paste? :)




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