Sciencemadness Discussion Board

Making ethanol at home.

Roachburn - 8-11-2011 at 08:39

I saw a video about making ethanol from sugar and corn meal and thought that this would be fun to do at home. I think it is a good project for budding chemists wanting to practice distillation. I didn't find a thread with this topic other than what information is scattered across multiple pages on these forums. So I decided to start one here. Here are some questions I was hoping to answer. What steps can be taken in order to maximize alcohol yield? Does temperature matter? What other types of sugar can be used aside from table sugar? What else can you use besides cornmeal? How do you know when the conversion is complete? Airlock substitutes? I am doing the cornmeal method, but I also want to try potatoes. Information on other recipes would be great! I made a few different types of air locks so I can post pictures for others to see how those are made.

ScienceSquirrel - 8-11-2011 at 08:50

The best way to make ethanol at home is from sugar and turbo yeast as you can get a wash of about 20% to distill.
This is a lot higher than any grain or fruit based liquor could go with conventional yeast.
Bugger, I forgot the link :(, it must be feeding time!

http://turbo-yeast.com/

[Edited on 8-11-2011 by ScienceSquirrel]

Roachburn - 9-11-2011 at 00:25

Turbo yeast would definitely be the most efficient way so it seems. The price isn't too bad either. I wonder if any of the brewers in town would sell me some. That would probably be even cheaper then to ship some. Originally I hadn't planned on making drinkable ethanol but the more reading I do I think it would be fun to brew some beer or good tasting liquor. Either way I need to get me some of this yeast ! The batch I have going now will be for my alcohol stove. Hopefully it will be done by tomorrow. I started it on the 4th. Should yield at least 8% I hope from what I have read. Also, does anyone know if light is good or bad for the fermentation process?

Roachburn - 9-11-2011 at 00:34

By the way does anyone know if you have to get a license to brew your own beer and such in the USA? Or is it legal?

ldanielrosa - 9-11-2011 at 02:41

My knowledge may be outdated, and laws vary from state to state but- I think the yearly limit for home use without a license is 50 gallons of beer, cider or mead (or combination thereof) for a single adult household or 100 gallons for multiple adult household.

Distillation is a lot touchier than brewing from a legal standpoint.

Choose the yeast for the application. If it's been optimized for high alcohol tolerance then it's use for consumables may have been compromised.

[Edited on 9-11-2011 by ldanielrosa]

Fusionfire - 9-11-2011 at 02:57

In the UK you can apply for a licence from HMRC to buy denatured ethanol (containing denatonium chloride). The licence is usually issued without a fuss for small quantities (tens of litres). I bought 10L of it from a supplier after getting the licence.

Apologies if you are looking into making ethanol at home purely for the experience of doing so :)

Lambda-Eyde - 9-11-2011 at 03:26

Beware that you need a good column, a lot of patience and preferably a large round bottom flask (3-5 L) if you're going to use ground glassware. When doing 10 L of mash, you need to distill like 15 times with a 1 L flask, and after that distill the 2-3 L of impure alcohol slowly through a good column. Last time I did it I tried both a 36 cm vigreux column and a 30 cm hempel packed with SS scrubber pads. Both resulted in a product consisting of 87% alcohol according to densimetry, with a noticeable unappealing smell. I'm going to invest in a longer hempel (60 cm) and distill more slowly, hopefully giving a clean product at >95%.

ScienceSquirrel - 9-11-2011 at 04:10

You can buy turbo yeast in small packets from home brew shops. It needs a low temperature to start, around 15C, as it makes so much heat itself.
This is a UK supplier but a quick Google will find suppliers elsewhere.

http://www.the-home-brew-shop.co.uk/acatalog/High_Alcohol_Tu...

If you want to make beer you need a good beer yeast. My favourite is this one.

http://www.the-home-brew-shop.co.uk/acatalog/Safale_S-04_Eng...

A good wine yeast is essential for making drinkable vino.

Arthur Dent - 9-11-2011 at 04:53

There is an art in the knowledge of what's calledf foreshots, heads and tails... Distillation of a fermented mash contains Ethanol as well as all sorts of nasties like Methanol and Acetone. When you begin the distillation of a mash, the very first stuff that starts coming up, called the foreshots, are low-boiling point poisonous chemicals that aren't useable for anything and contains little or no ethanol. You must discard this.

Then when the ethanol starts coming up in the still, it still contains some of these "nasties", in distiller's lingo, they call this "heads". You can keep this portion of the distillation process but only to add it to a subsequent mash to increase the ethanol content.

Then you have the middle run... after the foreshots and heads, this is the part that you wanna keep as it is the clean ethanol/water azeotrope that will be later refined further.

And towards the end, you have the "tails", which contains Ethanol, as well as higher-boiling aromatic compounds that gives the yucky taste and smelly aroma to your distillate. Again you can keep some to add later to a subsequent mash, but when the boiling temperature starts increasing fast, now's the time to discard the rest of the mash, which is mostly water, gunk, proteins and olis.

The "art" comes when you get a hang of when do heads, middle and tails begin. You bottle your distillates in separate containers and label them with the alcohol content and the distilling stage, and further refine them when you're starting to have a good quantity of strong spirits.

It's a multiple stage process that can be very long and tedious if you use small glass labware. A good homemade copper still is a wonderful thing and can speed things up tremendously depending on size and style.

Remember that distilling entails boiling hydrocarbons and highly flammable solvent vapors. No open flame anywhere and make sure any vapor is vented or collected away from the heat source.

I'm due to prepare a small batch of energetic spirits in the next few days. i'll take a pic of my glass still... Very basic and slow but does the job.

Robert

fledarmus - 9-11-2011 at 11:55

If you are in the US this might be helpful. It is the ATF's view on what is legal for homebrewing. States also have their own rules, however, and you might want to check this site as well.

In short, the US allows you to make 200 gallons per multi-adult household or 100 gallons per single-adult household of beer or wine, and you can't distill without a permit. In Connecticut, the state only allows 100 gallons per multi-adult household or 50 gallons per single-adult household.

textex - 9-11-2011 at 12:07

Quote: Originally posted by Arthur Dent  
There is an art in the knowledge of what's calledf foreshots, heads and tails... Distillation of a fermented mash contains Ethanol as well as all sorts of nasties like Methanol and Acetone. When you begin the distillation of a mash, the very first stuff that starts coming up, called the foreshots, are low-boiling point poisonous chemicals that aren't useable for anything and contains little or no ethanol. You must discard this.


I pretty agree with ya that foreshots aint mutch usable for drinking, and it gives ya a nasty hangover, but that it consists of poisonous chemicals for the most part? In my younger years i have fallens asleep from my still a few times and gotten the foreshots with the rest of the batch, but i havent noticed any special ill effects. (A pretty safe, but not very good reflux still. Wouldnt have been running a still where a tube snapping could fill my house with ethanol vapour while tired.)

My experience aint any scientific proof thought, so would be fun to see if anyone analysed the levels of the other low boiling chemicals in it.

[Edited on 9-11-2011 by textex]

And to the OP, if you are gonna make a drinkable ammount of spirits, i woulda invested 100-400$ in a copper/stainless steel still. Depends on how handy ya are though. Some welding or silver soldering will necessary.

When it comes to the wash you want to use a good turbo yeast and sugar. Make sure to keep everything clean, and get a hydrometer to measure the alcohol content and when the wash is done fermenting.

The higher the fermenting temp goes, the faster it will usually go. Upto the point where the yeast dies ofcourse(around 30-40 degree celcius) Remember that the yeast produces some heat itself, so theres no need to keep the fermenting bucket in a warmer room than 20-25 degrees. The yeast usually produces some more fusel oils when you ferment it fast.

When it comes to the sugar i usually add 6-7 kg of sugar and top the fermenter up too 25liters with water. If i remb correctly this gives me a alcohol content on around 13-14%. You can add up to 8-10kgs, but it will take more time, and you risk that the yeast dies without having fermented all the sugar which can give you some sugar residue in the still after boiling it. The quickests yeasts use around 2-3 days to ferment 6 kgs, more than that takes upto 1-2 weeks .

If you wanna drink it, it might also be worth letting it stand a week or use some enzymes to make the dead yeast fall to the bottom so you can separate it off. I've also heard some talk of using a small ammount of KMnO4 to oxidise some of the fusel oils or something like that.

[Edited on 9-11-2011 by textex]

watson.fawkes - 9-11-2011 at 12:43

Quote: Originally posted by textex  
I pretty agree with ya that foreshots aint mutch usable for drinking, and it gives ya a nasty hangover, but that it consists of poisonous chemicals for the most part?
Typically the foreshots contain large amounts of methanol, which is plenty toxic. The thing is that ethanol ingestion is one of the main treatments for methanol poisoning. (It pushes methanol catabolism onto an alternate pathway that's far less toxic.) So when you drink hooch not overly contaminated by foreshots, it's usually not fatal.

Compounds likely to be found in foreshots: acetaldehyde, acetone, methanol, and ethyl acetate. All these have lower boiling points than ethanol and, to boot, form low-boiling azeotropes with a number of other species in the mash, such as higher 3-5 carbon alcohols, other aldehydes such as fulfural, and other esters.

textex - 9-11-2011 at 12:56

Still i'd like to see some references saying that the foreshots contains a large ammount of methanol. I read a bit about it on a brewing forum im on, and i see that a few members there(prolly alcoholics ;D) that has been drinking pure foreshots they have been collecting in a day of need.

Should also be said that i heard of alot of methanol poisonings, but never any from any kind of homebrewing, just from greedy f*ckers "watering" their stuff out with methanol cause its cheaper.

Neil - 9-11-2011 at 14:37



You certainly want to toss your tops and bottom(as mentioned) but you also want to feed the yeast as clean a meal as you can.

Complex things like red grape juice yield a 'dirtier' brew then say, pure corn sugar. The more things there are for the yeast to gobble the more waste products they will make that are not ethanol.


This site has just about everything...

http://homedistiller.org/#safety

DougTheMapper - 10-11-2011 at 07:44

This topic has been discussed ad infinitum:

http://www.sciencemadness.org/talk/viewthread.php?tid=7379
http://www.sciencemadness.org/talk/viewthread.php?tid=8095
http://www.sciencemadness.org/talk/viewthread.php?tid=17496
http://www.sciencemadness.org/talk/viewthread.php?tid=13809
http://www.sciencemadness.org/talk/viewthread.php?tid=15300

And finally:

www.google.com

Hennig Brand - 11-11-2011 at 08:09

Does anyone know if there are any significant chemical changes to the Mash or Distillate during the distillation of ethanol?

I have always been under the impression that distillation of ethanol is for the most part simply a chemical separation process and that chemical change is negligible. I have noticed that many lay people believe that the toxic chemicals they associate with home distilled liquor are produced during the distillation. I always tell them that the composition of what is to be distilled is determined during the fermentation process and that the distillation merely concentrates and purifies the desired components of that mixture.

Have I been misrepresenting what is actually going on in any way?

ScienceSquirrel - 11-11-2011 at 08:17

Most of the congeners are formed from minor constiturents that are also present in the substrate by fermentation.
Some of them are toxic eg the higher alcohols like fusel oil and some add important flavours and aromas to the finished drink eg brandys and whiskys.
A lot of drinks like gin and vodka rely on a pure alcohol base that is then flavoured and or diluted with spring water to bottling strength.

gutter_ca - 11-11-2011 at 11:13

IIRC, the large amounts of MeOH in moonshine come from using a wooden mash pot.

textex - 11-11-2011 at 11:35

I think your pretty mutch right there hennig. I think most most cases of people getting ill from moonshine (apart from the ethanol itself) comes from people taking shortcuts when making their still. Like using condensors containing lead or using galvanized pipes/valves they found in the shed etc. Here in the country where the cheapest litre bottle of vodka costs 40$ we also had some cases where people bought E85 fuel, to remove the gasoline selling it in cartoons.

[Edited on 11-11-2011 by textex]

Hennig Brand - 11-11-2011 at 12:07

@textex
I just noticed your post after writing this one, as you can see I agree with you.

I think a lot of the unreasonable concerns over homemade liquor come from the old days when selling moonshine was a big thing and very ignorant and/or unscrupulous people were involved in the trade.

I have heard of people using car radiators to condense the vapours from the still. They were often not very careful about getting all the antifreeze out of them before putting them into service as condensers which often contaminated the distillate with ethylene glycol. Also in the radiators was lead which contaminated the distillate. Lead and other poisonous materials were also often used in still construction.

The biggest reason for contaminated liquor as far as I can tell was from greedy business people with no regard for other people's well being. Many different chemicals, all of which were cheaper than ethanol, were routinely added to moonshine in order to boost profits.

Why would the hard liquor be any worse for you than the beer or wine it was made from? As far as I can tell it isn't, unless of course you managed to concentrate the more poisonous fractions and then insisted on drinking them, or were very foolish and didn't know the difference. Even if you did manage to not separate and discard the more poisonous fractions when distilling I think the amount of methanol and other toxins formed from a normal fermentation is very, very small relative to the amount of ethanol. The metabolism of ethanol and methanol and many other toxins are competitive processes in the human body, so if there is a much larger quantity of ethanol, the toxic effects from the contaminants will be much less.

I have actually heard that it is, or was common practice to get a patient to drink large amounts of ethanol if the patient had consumed methanol or ethylene glycol.

It is probably hard to make a Scotch Whiskey that tastes the same as what is bought from the store. I think it is possible to make good Vodka without much effort, and all other liquors are basically just adulterated Vodka anyway ;).

I really don't think homemade liquor should be all that dangerous. In my opinion, most of the negative attention toward home made liquor comes from it interfering with tax revenue.



[Edited on 11-11-2011 by Hennig Brand]

S.C. Wack - 11-11-2011 at 17:59

Quote: Originally posted by Roachburn  
...potatoes...


Gattermann has this. I remember this now, but sadly not when met with a nearly-free, perfectly-sized, but rather heavy SS autoclave.

Screw the copper, alembics, terminology, and all.

Hennig Brand - 13-11-2011 at 07:22

@Roachburn

With regards to using airlocks during fermentation, when using turbo/super yeast and sugar to make alcohol, I have always just used a bucket with a loose-fitting cover. Carbon dioxide (CO2) is more dense than air and will form a protective blanket over the fermentation as long as the fermentation is fairly vigorous (fermentation produces CO2 as you know). Within a day or so of fermentation completion the mash is distilled. If I was going to hang onto the mash for a while, I would use the loose-fitting cover during the primary vigorous fermentation period, and then install an airlock.

As far as I know light is definitely a bad thing, causing degradation of your beer or wine. Mostly pure ethanol (distillation product) is much less affected by light as far as I know.


BTW, success when making alcohol (fermentation) is often quoted as being ~80-90% about getting your fermentation vessel and anything else the mash comes into contact with clean and disinfected (free of bacteria and other yeast).



[Edited on 14-11-2011 by Hennig Brand]

Arthur Dent - 14-11-2011 at 04:54

Quote: Originally posted by Hennig Brand  
... I have always just used a bucket with a loose-fitting cover....


Hi Hennig,

I've done the same for many years, it is indeed enough in many cases, but since then, I have been doing this in a place that needs a controlled environment, so the gases and aromatics released by fermentation have to be captured somehow. I perform my brewing endeavors in my work area, which is basically a bedroom in my basement converted into Dr. Frankenbob's Lab! That's the reason behind the elaborate gas scrubbing apparatus during fermentation and distillation.

As for light, I agree, no need for total darkness, but indirect incadescent light and nothing from sunlight is okay I guess.

And finally for the cleaning, a dilute bleach solution is indeed perfect to sterilize the beer bottles, which are rinsed with cold water and let to dry on an improvised drying rack (washing machine's plate drawer). I used to buy the pink food grade powder bleach at the wine-making store, but found that plain old diluted bleach does an even better job. Over the years, and probably a total of 40/45 batches of beer succesfully bottled, only one went bad... I can only describe the cascade effect of a runaway fermentation in a case of 24 beers! Yikes!!!!

Robert


smaerd - 14-11-2011 at 07:26

Does anyone know what a good OTC source for nutrients aside from sugars would be for yeast culturing?
Quote:
Yeasts also have a requirement for phosphorus, which is assimilated as a dihydrogen phosphate ion, and sulfur, which can be assimilated as a sulfate ion or as organic sulfur compounds such as the amino acids methionine and cysteine. Some metals, like magnesium, iron, calcium, and zinc, are also required for good growth of the yeast.

from - http://en.wikipedia.org/wiki/Saccharomyces_cerevisiae

I see that a lot of people simply throw yeast, water, and sugar together and it turns out okay ethanol production-wise, but I've also read in journals of people using soybean/glucose media(iirc). Just wondering if anyone had any tips for healthy culturing.

Hennig Brand - 15-11-2011 at 13:24

Hi Arthur,
Sounds like you have a good set up there. I have only made beer 4 or 5 times now, but it all turned out fairly well. The very first batch wasn't quite as good because my fermentation temperature was quite high and fluctuated a fair bit. I soon discovered ways of keeping the fermentation temperature where I want it and constant (a cool room, a water jacket and a good thermostatically controlled aquarium heater for the water in the water jacket). I learned that the beer tastes much better when the fermentation temperature was kept down and constant. I guess different beers/yeasts probably have different temperature requirements though.

A friend of mine who was starting out had 2 batches of beer in a row go bad on him because he thought all the cleaning and sterilization was excessive and unneeded.

I have also made wine a few times but most of my experience comes from fermenting sugar, molasses and other things for distillation purposes. I always found distillation very interesting. I started out distilling other people’s homemade wine, which probably turned me into a hobby chemist/experimenter. It might have been the black powder I made when I was 10 that started the chemistry/fire fanaticism (the black powder wasn't very good quality).


@smaerd
Most of the main chemical nutrients used for brewing are the same salts found in common fertilizers, like ammonium phosphate, ammonium sulphate and others. The fertilizers typically are not food grade, which is something to keep in mind. Any of the brew shops will either have or be able to order in for you whatever nutrients you want. The last time I looked at a 1lb bag of ammonium phosphate at a brew shop, I remember thinking that I could buy a 50lb bag of fertilizer grade for about the same price. The truth is that most people need very little of these nutrients unless they are doing a lot of brewing, which is why I didn't bother with the fertilizer.

BTW, the super/turbo yeasts are a mixture of yeasts and nutrients designed to produce a higher than would normally be possible concentration of alcohol. Since all the nutrients are included in the package all you need is refined sugar and water. Without the added nutrients fermenting pure sugar water would be the same as a human trying to live on refined sugar. Unrefined sugar actually does have a lot of nutrients in it for the yeast. Anyway, the simplest thing is probably going to be to buy a package of super yeast.

ScienceSquirrel - 15-11-2011 at 16:32

Turbo yeasts are strains that will tolerate very high sugar and alcohol concentrations plus the packs do contain the nutrients needed to supplement the water and sugar washes that are used with these strains.
Beer yeasts are bred to operate in the 4 - 12% range in a hopped wort, most wine yeasts can handle 8 - 15% in a fruit juice derived liquor.
Turbo yeast can go as high as 23% with only sugar, water, a nitrogen source and some vitamins.

byko3y - 25-4-2015 at 19:45

I've tried to make a small amount of ethanol from sugar, and I succeeded (got 100 ml of pure ethanol), but the problem is - how can I get rid of a horrible smell of fermentation process?
The first man that comes into my apartment can tell that I'm making ethanol here, or at least he will ask if I keep a dead body in my wardrobe.

Zombie - 25-4-2015 at 21:32




[Edited on 4-26-2015 by Zombie]

[Edited on 4-26-2015 by Zombie]

byko3y - 26-4-2015 at 11:09

Substitute one horrible smell with another? Are you sure?

Zombie - 26-4-2015 at 19:07

Positive.

One night I met a Gal in a bar... never mind.:P

macckone - 27-4-2015 at 19:07

Make sure your fermenter vents out a window. That is what they make vinyl tubing for. Good mash smells like a bar at closing time. If it smells like dead people, piss or vomit then toss it, or find a new bar.

byko3y - 27-4-2015 at 19:19

I started a new mash fermentation, this time I used an improvised reflux condenser made out of glass tubes.
And you know what? I can barely feel its odor. Most likely there was some high boiling stinky stuff which gave the odor first time.

byko3y - 6-5-2015 at 06:29

Got some sad news: I failed to distill any ethanol after 6 days of fermentation. But I've got (from 2L total volume) 70 ml of isopropanol, and a hell lot of amyl alcohols and other higher alcohols. Who have drunk all my ethanol?
I'm not sophisticated in brewing, is the only possible reason for the absence of ethanol is aerobic fermentation leading to acetic acid? But when I tried to mix the fermented product with baking soda, I got only slight bubling, much weaker than that of 5% acetic acid solution.
Did I fail fermentation, or maybe used some wrong nutrition, or wrong distillation process if the only possible reason?

Zombie - 6-5-2015 at 07:17

Explain what you used to ferment, the yeast, and or nutrients, and the conditions in which you fermented... Container? temp? dark? light?

Did the ferment bubble actively?

What did you ferment, and the recipe?

What was your distillation process? how much distillate did you recover from how much "beer"?

What were you wearing? ;)

Amos - 6-5-2015 at 07:22

If you're trying to make ethanol by ANAEROBIC fermentation with yeast, then first step is to exclude any and all oxygen! You shouldn't have any worries about aerobic oxidation to acetic acid if you made an attempt to air-lock it.

byko3y - 6-5-2015 at 07:42

I'm using regular OTC baking yeasts, have no idea about what is the species name.
I made a mash from 1.7 L of water, 400 g of inverted sugar (obtained by heating a sugar at 80 C with 1 g of citric acid), 1 g of urea, 10 mg of B2 vitamin (it was a B-group vitamin complex in fact), 2 g of Ca3(PO4). The temperature was maintained 27-30 C all the time after making the above solution. When I added the yeasts, bubbling started pretty rapidly, and it was bubbling for 2 days, than intensity decreased, but there was still some bubbling, so I decided to keep it fermenting for 5 more days.
About fermentation device setup: it was a 2L bottle with 29/32 joint, in which was inserted a tube 20 cm long, plugged with a cotton wool.
On 7th day I replated the plugged tube with a usual glass air-lock device (like this one ), cooled, and let it settle for few hours. Then I decanted everything except bottom layer and distilled it. The first fraction that came off the distillation column was 80 C+.
This was the lowest fraction I managed to separate, which is isopropanol (checked by iodoform test).

Zombie - 6-5-2015 at 07:54

It all sounds right. You should have recovered around 200mL ish of EtOH. @ approx 40-50ABV

Did you use a water cooled condenser?

byko3y - 6-5-2015 at 08:44

My apparatus was similar to this one , in case you don't see the picture: source flask (one neck), fractioning column, three-way adapter with thermometer, water-cooled liebeg condenser, receiving adapter.

Zombie - 6-5-2015 at 10:18

The way I see that set up, the calcium chloride is supposed to dry the ethanol but in its position it can not. Nothing would be recovered there.

The calcium chloride filter would have to go either in the vapor path before condensing or in the condensate path before collection.

You would also need to monitor the ABV of the condensate or the head temp at the top of the column to know when to stop collecting.
The head temp should remain steady at whatever number thru the majority of the run. Once you see a gradual rise in temp... it is time to stop distilling.

I hope some of this applies...

[Edited on 5-6-2015 by Zombie]

Amos - 6-5-2015 at 13:14

I don't know about all those vitamins and nutrients you added, or why you would use inverted sugar. I make my ethanol with quite high yield from simple table sugar, water, and turbo yeast. Works great every time, and the mixture concentrates to about 17-18%.

Metacelsus - 6-5-2015 at 14:54

Yes, yeast expresses sucrose invertase, so there's no need to invert the sugar - it does it for you.

@Zombie: Calcium chlorate? Do you mean chloride?

Zombie - 6-5-2015 at 15:03

Yes.

I hope I didn't turn his lab into a roman candle...

I'll go back, and edit that... THANKS!!!!!

Zombie - 6-5-2015 at 15:07

Quote: Originally posted by Amos  
I don't know about all those vitamins and nutrients you added, or why you would use inverted sugar. I make my ethanol with quite high yield from simple table sugar, water, and turbo yeast. Works great every time, and the mixture concentrates to about 17-18%.



I recognize the formula. It was originally posted by a fella called Punkin on the distillation forums.

They tend to over think the simplest things there. Booze, free time, nonsense.

byko3y - 6-5-2015 at 16:35

Receiving flask was the last in my apparatus, no calcium chloride tube was present. Sorry, I was lazy to edit the picture and post it here.
I see all over the internet articles and some people recommend to invert the sugar before adding it to a mesh, though I was not able to find an answer about why shoul I do the same. They say that yeasts more easily consume inverted sugar, while they have to invert the regular one.
Ammonia leads to lesser amount of higher alcohols; vitamin B2/olive oil/small amount of oxygen is needed for yeasts reproduction.

[Edited on 7-5-2015 by byko3y]

Lambda-Eyde - 8-5-2015 at 04:39

Quote: Originally posted by Zombie  
The way I see that set up, the calcium chloride is supposed to dry the ethanol but in its position it can not. Nothing would be recovered there.

It is not supposed to dry the alcohol, it is supposed to prevent ingress of humid air into the apparatus. This is a pretty common usage of a drying tube. Calcium chloride can't be used to directly dry simple alcohols anyways.

byko3y - 8-5-2015 at 10:58

Today I tried a carefull distillation with H2SO4 added into the fermentation product. Ethanol was distilling ri-i-i-ealy slow at 78-79°C, but after all, I've got a clear liquid with 0.80 g/ml density, most of which is probably a 96% ethanol, 55ml of a semi-pure product from 550ml of crude one.
After destroying esters with sodium hydroxide and another distillation, I finally got something like 45 ml of pure ethanol boiling at 78.2-78.8°C.
Maybe I tried to distill too rapidly in my previous try, and the fractioning column failed to separate ethanol and isopropanol, which have close boiling points (78.3 and 80.4). I can extrapolate the numbers, claiming 150 ml of 96% ethanol yield from 2200 ml of total product volume, which is 7%. I was sure the regular yeast could give at least 12% :( Gonna try a high load of a regular sugar next time.
Also, I was stupid to perform haloform test on the ethanol, because both ethanol and isopropanol give positive result, so you can't use the test to differentiate them.

blogfast25 - 8-5-2015 at 12:13

Quote: Originally posted by byko3y  
I can extrapolate the numbers, claiming 150 ml of 96% ethanol yield from 2200 ml of total product volume, which is 7%. I was sure the regular yeast could give at least 12% :( Gonna try a high load of a regular sugar next time.


Why did you add H2SO4 to the fermented mash?

Did you measure alcohol on what was left in the pot?

Did you allow fermentation to finish completely?

1 mol of glucose (180.16 g) yields 2 mol ethanol (2 x 46.07 g) of ethanol.

For 12 w% EtOH (normal yeast), start with 235 g sugar per litre of mash. That's what I used to do, worked a treat. Allow 2 weeks or until bubbling stops. Use a wine hygrometer or refractometer for ABV.

You're not easily going to detect small amounts of IPA with chemical tests.

[Edited on 8-5-2015 by blogfast25]

byko3y - 9-5-2015 at 01:47

I dunno why I added H2SO4. I was hoping it will help to break esters and other shit. Not really sure if it helped.
Yes, I allowed the fermentation to finish. I measured the 55 ml volume using a graduated cylinder.
After full oxidation primary alcohols convertinto acids and IPA converts into ketone. You can use acidic fuschin then (schiff's reagent) to detect the acetone. Or nitroprusside (rothera test), which is more specific to ketones. Anyway it requires some separation of oxidized products from the mixture, so it's a lot of work.
And thanks for explaining stochiometric proportions, I was wondering about those proportions, because all over the internet people post weight proportions, and in fact it's all about 1:2 moles.