Sciencemadness Discussion Board - Unidentified blue oil in ethanol.

Unidentified blue oil in ethanol.

anolog - 30-1-2015 at 13:10

Hello l made ethanol from yeast and sugar l fermented it for two days, then l distilled it and l got about 30 ml of crude ethanol then l added 2 tablespoons of copper sulfate to it and l let it sit for 2 hours, then l filtered the liquid and it had this light blue color, then l added 1 tablespoon of sodium carbonate to it and the powder turned to slime and on top of the slime formed this dark blue oily liquid, l let it sit for 2 hours and l filtered it. Now l have this odd liquid with two layers, it is very flammable.
The whole liquid is oily in water.

Zombie - 30-1-2015 at 13:31

You must have had ammonia in the ferment. Copper will react with ammonia to make Schweizer's reagent ( tetraamminediaquacopper dihydroxide ). You must have had a high PH, and some sort of yeast nutrient.

Where ever it came from there was ammonia present in the ETOH.

Volanschemia - 30-1-2015 at 15:25

Is the oil miscible with the Ethanol?
If it isn't you could just remove it with a sep funnel or decant it if you don't have a sep funnel.

If it is Schweizer's Reagent you can destroy it by adding some acid (usually Sulphuric Acid to form Copper(II) Sulphate again).

I'm doubtful though whether Schweizer's Reagent could from with Copper(II) Sulphate and in such a dilute solution of ammonia.

Going off your post, I gather the oil only formed when you added to Sodium Carbonate? If that's the case then you would have formed Copper(II) Carbonate which could possibly react with ammonia but I'm still doubtful that it could form in such a dilute solution.

Does your ethanol smell like ammonia?

blogfast25 - 30-1-2015 at 16:13

Quote: Originally posted by anolog

Hello l made ethanol from yeast and sugar l fermented it for two days, then l distilled it and l got about 30 ml of crude ethanol then l added 2 tablespoons of copper sulfate to it and l let it sit for 2 hours, then l filtered the liquid and it had this light blue color, then l added 1 tablespoon of sodium carbonate to it and the powder turned to slime and on top of the slime formed this dark blue oily liquid, l let it sit for 2 hours and l filtered it. Now l have this odd liquid with two layers, it is very flammable.
The whole liquid is oily in water.

2 days? A normal fermentation requires at least 2 weeks to run to completion, yet you claim to have obtained 30 ml of crude ethanol after distillation... A 750 ml, 12% ABV bottle of wine contains only 90 ml of pure ethanol, so how much of your part-fermented sugar water did you have to distil?

Also, why on Earth did you want to add copper sulphate to that?

[Edited on 31-1-2015 by blogfast25]

Zombie - 30-1-2015 at 17:45

there are several things that come over in distillation The very first are acetone, and keytones. That is what distillers call fore shots. Next is ETOH in reducing ABV, and third are what we call tails or fusel oils such as propanol, butanol, and amyl alcohols.

The tails are easily identified by their oily appearance, and foul smell. They also do not readily separate from ETOH but can be re-distilled to remove them.

I'm gonna stretch here for a moment, and assume you used a "Turbo yeast" or nutrient enhanced yeast. That's the only way to complete a ferment in 48 hours. That would be where the ammonia came from.

Pardon my assuming here but it would explain everything except some of the questions about yield, and why add compounds after distillation.

You can re'run your product, and clear the oil, and color. As to what the additional chemicals have done or will do... I leave that to the smarter fellas here.

Oh yeah... The acid... Yes acid will help clear the blue. I use Citric acid as it is cheap, and easy to find here. About 2 grams to a gallon before re distilling.

[Edited on 31-1-2015 by Zombie]

blogfast25 - 30-1-2015 at 17:55

Quote: Originally posted by Zombie

I'm gonna stretch here for a moment, and assume you used a "Turbo yeast" or nutrient enhanced yeast. That's the only way to complete a ferment in 48 hours. That would be where the ammonia came from.

Pardon my assuming here but it would explain everything except some of the questions about yield, and why add compounds after distillation.

Show me any evidence that turbo yeast can complete fermentation in 48 hours and that it generates ammonia.

Even the most devious of turbo yeast marketers don't make that 48 h claim. I'm a home brewer too.

For the copper tetrammine complex to form, you need quite a bit of ammonia, as the alkalinity first precipitates the copper as Cu(OH)2, which is very insoluble and only dissolves in an excess NH3.

[Edited on 31-1-2015 by blogfast25]

Zombie - 30-1-2015 at 17:59

I'll see your 48 hour yeast, and raise you 24 hours...
The key ingredient that makes them "Turbo" is ammonium nitrate. or Miracle Grow.
Thus the ammonia

Just an assumption that he used any...

I don't brew, I distill. We refer to Turbo products as Fuel Yeast. The off flavor compounds must be carbon filtered out. Thus my assumption. I could be wrong.

http://www.amazon.com/Alcotec-24-hour-Turbo-Yeast-grams/dp/B...

[Edited on 31-1-2015 by Zombie]

blogfast25 - 30-1-2015 at 18:04

Well, I suppose he'll own up to using turbo crap or not.

I'm deeply sceptical with regards to 48h claims, ammonium nitrate or not. Just because it says so on the packet doesn't make it true.

[Edited on 31-1-2015 by blogfast25]

Zombie - 30-1-2015 at 18:18

I actually 100% agree BUT... I have used miracle grow to rekindle stalled ferments, and had them finish off in a day.
The 48hr stuff I tried several years ago actually did finish 55 gallons of molasses wash in 3 days BUT you could smell the ammonia in the beer, and it turned my ETOH blue. That's how/where I learned this.
The blue came from the copper plumbing, and the Citric acid cleared the second run thru.
Due to the smell, it wound up as weed killer along the fence line.

radiance88 - 31-1-2015 at 02:03

From my very limited understanding, you are supposed to clean out your copper pipes before every run or risking contamination from the residue inside your pipes. I've seen this done using white vinegar (acetic acid), and I'd guess you could use some similar weak acid thereof..

You'd be able to observe this as the vinegar distills through your column/coil, you get a blue colored solution which is otherwise what you'd risk contaminating your batch with.

My guess is somehow since you have a blue colored solution, you have gotten some kind of copper compound into your solution from gunk built up inside your copper tubing..

-------------------

After re-reading your post, I would have normally said the above.. but you added copper sulfate to your solution - what was the purpose of adding that? This is the first time I've ever heard of that being done.

[Edited on 31-1-2015 by radiance88]

Zombie - 31-1-2015 at 02:43

Yeah. It's a little off topic but still relevant.

Part of the fermentation process releases sulfites (SO23). This is carried in the distillation vapor right thru to the condensed product, and yes sulfites are found in most every plant that is used in fermentation, including sugar. More so in fruits, and grains.
Distillers use at least SOME copper in the vapor path for one reason only. To bond the sulfites to the copper, and remove them before condensation.
This reaction actually turns the copper a dark brown as it accumulates. It will never actually release from the copper but instead it causes a reaction that gradually eats away the copper.
So long, and short of it is it does not turn ETOH blue. That is a different reaction.

Also you are correct that acid (vinegar / citric / ect... will remove the sulfites from copper.

I only posted this for the clarity of the thread.

radiance88 - 31-1-2015 at 04:26

Quote: Originally posted by Zombie

Yeah. It's a little off topic but still relevant.

Part of the fermentation process releases sulfites (SO23). This is carried in the distillation vapor right thru to the condensed product, and yes sulfites are found in most every plant that is used in fermentation, including sugar. More so in fruits, and grains.
Distillers use at least SOME copper in the vapor path for one reason only. To bond the sulfites to the copper, and remove them before condensation.
This reaction actually turns the copper a dark brown as it accumulates. It will never actually release from the copper but instead it causes a reaction that gradually eats away the copper.
So long, and short of it is it does not turn ETOH blue. That is a different reaction.

Also you are correct that acid (vinegar / citric / ect... will remove the sulfites from copper.

I only posted this for the clarity of the thread.

Thanks for the information Zombie. As always, this stuff is -very- fascinating.

I guess this relative lack of knowledge comes from me pretty much watching all these moonshine videos on YouTube. Building my own still is actually my current project underway. Hell, most of them do not even mention that you have to add something that contributes amylase enzymes to your mash/wash when using corn and other plant products - most of them just assume that it will all magically convert to alcohol.

Zombie - 31-1-2015 at 04:44

PM me or post a thread if you want help designing a still.

Sorry for sidetracking the thread Anolog...

[Edited on 31-1-2015 by Zombie]

blogfast25 - 31-1-2015 at 08:16

Quote: Originally posted by Zombie

The 48hr stuff I tried several years ago actually did finish 55 gallons of molasses wash in 3 days BUT you could smell the ammonia in the beer, and it turned my ETOH blue.

If the level of NH3 is so high you can smell it then formation of copper tetrammine cations in the presence of CuSO4 is highly plausible, no contest there.

The OP needs to run a paper pH on his distillate and a smell test.

BTW, sulphites are noted as salts of sulphurous acid: H2SO3. The sulphite ion is SO32-. This is a science forum, remember? Express yourself concisely.

[Edited on 31-1-2015 by blogfast25]

Zombie - 31-1-2015 at 10:04

I feared using h2so3 as the factual molecule due to its lack of characterization.
Truth of the matter is you are correct.
It is the vapor sulfurous acid that attaches to the copper.

Bert - 31-1-2015 at 11:05

Any reason (besides ease of construction & high thermal conductivity!) you don't choose less reactive materials such as stainless steel, glass and ceramics? Seems that plumbing store Copper coil brings some product purity issues...

Zombie - 31-1-2015 at 11:47

It's a double edge sword.
The copper is actually need to attract the sulfites. They are in all mashes/washes in different amounts.
It also goes back to the beginnings of distillation. They realized (somehow) that copper made for a cleaner product.
Distillers are a superstitious lot that tend to remain in the dark ages. Change is frowned upon.

Now the modern distillers are all using Stainless for lot's of obvious reasons. The wow factor, and the wear factor are tops. BUT they ALL have some copper in the vapor path. It is not needed in the boiler because sulfurous acid has not been found in dilution. Somehow they again new this, and only introduce copper in the vapor path to pull the gaseous acid.

Ceramics are just not thermally correct for the application. They retain too much heat, and respond to temperature changes too slowly. To control the quality of the product (ETOH) you have to control the evaporation rate. Heat or energy input is your only control there.

Some "home" style columns are going to glass but I think you can easily see the main issue there... ETOH + distiller + GLASS!!! Bad company.

My main attraction to distilling was formed around the chemistry. All this other jargon is new to me but process is not. All things have to happen mechanically.

Forgot the hardware store copper... It does have issues that MUST be addressed before consuming anything. The entire still has to be run three times. First is an acid run. Acetic acid (white vinegar) is the easiest. Diluted, and run with no condenser to saturate all the interior surfaces, followed by a "Junkahol" run Sugar wash w/ higher than normal ABV. That sort of seasons the stripped copper. Followed by a Steam run just to square it all up, and piece of mind.
After that it's party time till the copper wears out. (decades)

Sorry to jack your thread again Anolog.

[Edited on 31-1-2015 by Zombie]

Bert - 31-1-2015 at 12:32

Thanks. Never distilled anything potable- Been a couple of decades since I even made beer now.

Jacking a thread...

Jack... Jack... Jack... Applejack?

Mmm. Freezing the water out is sounding better & better.

(Edit)

Oh wait. "apple palsy"? WTF! Maybe not so good after all- Can't discard fore shot/after shot if you never distill-

[Edited on 31-1-2015 by Bert]

blogfast25 - 31-1-2015 at 13:33

Quote: Originally posted by Zombie

I feared using h2so3 as the factual molecule due to its lack of characterization.

Worry more about spelling than characterisation in this case. "h2so3" is txtinglish applied to chemistry.

Zombie - 31-1-2015 at 14:09

I give How the hell do you do that with the number thingys' and the alphabetaters. 10-4.

The thing you did to bounce the numbers around.

[Edited on 31-1-2015 by Zombie]

Bert - 31-1-2015 at 14:47

Quote: Originally posted by Zombie

The thing you did to bounce the numbers around.
[Edited on 31-1-2015 by Zombie]

To get the subscript/superscript options, hit "preview post". You will be offered several buttons for formatting that don't appear if you just do a quick reply- See image below:

Or if you wanna be a big 'ol cheater and steal some formatting you don't know how to do, but saw someone else use? Just hit "reply with quote", and then go look at the HTML used & copy...

[Edited on 31-1-2015 by Bert]

Zombie - 31-1-2015 at 15:54

]Thanks Bert. I'll have to re-read, and figure that out.
One thing I don't do is cheat. Either I get it right or I shoot the person bustin' my chops, and be done. (no witnesses)

I'm not bustin' on you BlogFast. I VERY much appreciate your help. I understand how valuable your attention, and time are. I appreciate you sharing to help me get better at something I am developing a passion for.
Hopefully in some way I can return the favor at some point.
Thank you both... :cool:

I think I follow... no, not yet. I'll get it tho. Maybe i'll cheat (sshhhh)

[Edited on 1-2-2015 by Zombie]