Home Distillation of Alcohol (Homemade Alcohol to Drink)

Distilling the Wash


Summary
Once the still is up to temperature, and the distillate has started dripping, make sure you throw away the first 50 mL per 20 L of wash, as this may contain any methanol that is present.

You should expect to collect the equivalent of approx 1L of 40% alcohol per kg of sugar used; the actual % purity will depend on the type of still you are using.

Stop collecting the distillate once you notice them containing some fusels, or if the temperature gets above about 94 oC (it doesn't become "dangerous" or "deadly", just that it tastes foul).

If you collect the distillate in small amounts (say 1/2 L or so), you can segregate the drinkable spirit from that with fusels in; the latter can be added to the next wash, and be collected cleanly then.

"Genuine" whiskey can be made by passing a grain wash through a pot still twice.


The alcohols in the wash begin to vapourise from the wash at specific temperatures. If by themselves they would be ...
(a mixture of several of them will be slightly different, however you get the basic idea). By tracking the temperature of the vapour, you have a fairly good idea when you're collecting the Ethanol your after (78-82 °C), vs when it is starting to get lean and you're into the higher alcohols.

Removing the Methanol

Be ruthless about tossing the first 50 mL (off a 20L wash) that you collect, as this contains any methanol (causer of hangovers - small quantities, or blindness - larger quantities). Even though I'm pretty sure I only collect less than 10mL at the methanol stage, I still discard 50mL, just to make sure. No need for penny-pinching when you're making 3L of the stuff, for less than $5.

This first portion is often called the "foreshots". They are different from the "heads". Ian Smiley (http://www.magma.ca/~smiley/main.htm) describes foreshots as "the low boiling point compounds that come out of the still first. They contain acetone, methanol, various esters and aldehydes, and other volitiles. Foreshots are to be considered poisonous and should be discarded." Whereas heads "come out after the foreshots, and are almost pure alcohol, except that they are contaminated with trace amounts of unwanted cogeners ..." To get a really clean distinction between the foreshots and the heads, first ensure that you've let your column equilbriate under total reflux, then hold the reflux ratio high, such that you remove the foreshots only very slowly (eg 1 drip per second), thus allowing an equilbirium to be maintained at the top of the column, encouraging the methanol to collect there.

If you're after making pure neutral spirit for vodkas or gin you may choose to keep the heads (eg the next 250 mL-1L of spirits) separate from the following couple of litres (middle run) on the basis of their taste. These heads can still be used to make liqueurs, whisky, rums, etc, or redistilled later if desired totally neutral. The only problem with heads is their non-neutral taste.

The distinction between the various phases depends on what sort of still you have. They will all tend to merge from one to the other. This is particularly the case with a pot still, where you notice the temperatures always slowly changing as the distilling run progresses. Using a reflux still or fractionating column will allow the various stages to appear more distinct, as the temperature will be more stable, due to the more distinct seperation of each compound.

When to Finish

The general rule is to finish distilling when the vapour temperature near the condensor is around 92-94 ° C. Depending on how much of the "tails" you collect, your spirits will aquire a different flavour. If making a neutral spirit, you wouldn't want any tails present, so you'd finish sooner, however if making a flavoured spirit, you'd want a trace of them present. Note that you can always collect the tails seperately from the "middle run", and redistill them at a later date to get the ethanol from them.

If you're doing a flavoured spirit, eg a schnapps or whisky, often the "cut" to finish will be based on taste rather than by temperature alone.

One clue that you've gone too far is if the distillate takes on a white/milky appearance. This is because the fusels (propyls, amyls & butyls) are partialy/totally insoluble with the higher %alcohols. You won't spot them if you keep your tails separate, as they are soluble within their own family in a weak ethanol solution. You may spot them though by seeing if a drop on the end of your finger gives a sun glint, and/or feels well lubricated (the old moonshiners trick). You may also see a slight film/slick on the surface of the distillate if using a clear container. If you can see them, then you can probably smell them too.

Another indication that its time to finish is when the temperature begins to fluctuate a bit. Tarvus writes :
Let the distillate drop cleanly into the recieving vessel, so that it splashes. This will help it lose any fusels that may be present. For the same reason, it is better that the distillate is still warm to the touch, not cold. Don't put the end of the tubing under the level of the liquid, as this will cause any fusels that are coming out as vapours to condense (and taint the flavour).

Greed is a bad thing. This is what gets your mates saying that your spirits taste "off" (you stopped noticing a while back, but everyone else still comments). You are either trying to rush things (good distillate requires time & patience), or you're wringing the neck of the beast and taking the run too far. You can't get ALL the available alcohol out of the wash. The better your still (eg the more "theoretical plates" / smaller HETP it has) the better your chances, but you still run the risk of contaminating your clean spirit with the tails, and having it smell & taste bad. But heres a few things to try ..
A 20L wash (at 12%) should produce approx 3L of 75% ethanol via a basic reflux still, or 2.3L of 95% ethanol via a fractionating reflux still.
L of wash at % alcohol
through a still that collects its distillate at %
should result in L alcohol collected
Note: this assumes 95% collection efficiency

Donald advises .. Mark has built a really neat device to allow him to monitor the alcohol purity during the course of the distillation. It floats a hydrometer in the distillate as it is received. Just remember to correct the readings for the higher temperature ....

You may be interested in something that I built so that I could monitor the quality of the output from my still. The device basically takes the output from the condenser and runs it past a hydrometer. I built this from a 6" length of 3/4 copper tube with a 1" tube flanged down and silver soldered at the top. I then connected a piece of 3/16 copper tube to the bottom of the 3/4 copper (input) and at the other end silver soldered on a funnel I then connected another piece of 3/16 copper to the 1" copper tube that collects the overflow from the 3/4 tube (Output tube). This connection was a little difficult as the 3/16 tube will not fit in between the 3/4 and 1" tube. To do this I drilled a small 1/8" hole into the side of the 1" tube and but welded it on. You could probably increase the 1" tube to 1.1/2" tube to make this easier The reason that the tube sizes are small is to ensure that the hydrometer can quickly follow any changes in output. A down side to the 3/4" tube is that if you have a high flow rate the hydrometer will give higher reading as flow of alcohol causes the hydrometer to rise. So if you are considering construction and you have high output rates you may need to increase the size of the tubes. This will of course decrease the sensitivity. I would also suggest to make sure that you hydrometer will fit inside of the 3/4" tube with some clearance for the output to flow past(My hydrometer is 1/2' diameter).

Salt

Maurice advises .. Salts are sometimes used during extractive distillation (eg when trying to distill past the 95.6% azeotrope) so as to depress the volatility of the water (eg effectively increase its boiling point, so you get a greater % of ethanol off compared to normal). Because the salt is non-volitile, it will always remain in the pot, and not turn up in the distillate.

The Household Cyclopedia recommends ...
David cautions though ..
Ken recommends using Sodium Carbonate to reduce the amount of fusel oils present ..

Boiling Chips

If you're heating your still over an external heat source, then you should have a couple of boiling chips inside it to help break the boil. These are any rough-surfaced, inert object - like bits of broken pottery (unglazed so as to avoid lead based glazes), broken glass, or even a couple of marbles.

The rough surface acts as a site where the bubbles can start to form easier. If your pot is nice and smooth on the inside, then its difficult for the bubbles to form, and you can end up super-heating the liquid. When it does boil, it might be quite violent, and give surges of vapour up the column, ruining that nice equilibrium you're trying to create. Boiling chips, although making the job a little noisier (rattle like hell!), do help give a smoother simmer.

Using a Pot Still

A pot still is fairly straight forward to use. Turn it on. Once the temperature is up to about 60 °C turn on the cooling water to the condensor. Make sure you throw away the first 50 mL per 20L wash, as this will contain any methanol that might be present. Segregate the distillate into 500 mL lots as it comes off. Only keep (for drinking) that which doesn't contain fusels (smell off) - probably below about 92 ° C, however you should keep distilling past here, untill about 96 ° C, as this fraction, although high in tails and not good for drinking this time, can be added back to the next wash and cleaned up OK then.

The Omnipresent Mecakyrios advises how he uses a Doubler with a pot still ... Jack writes ... Scrounge adds ...

Stripping

Pot stills can be used to "strip" the wash, prior to a reflux distillation. By passing the wash once through a pot still, it will be increased in purity from say 10-15% up to 40-60%, reducing it in volume by 1/5th. This way, you can strip say 100L of wash down to 20L of semi-clean spirit to then load into the reflux still for a single pass (rather than having to do 5 reflux passes of 20L of wash). This will not only save you plenty of time, but it will also help result in a somewhat cleaner spirit, as any yeast, etc get removed during the stripping run. You could also use a reflux still to do the stripping in, by simply not making it reflux any of the liquid.

Double Distilling for Whiskey etc

Here we try to replicate the traditional style as used in commercial distilleries world wide. See Making Whiskey - A Personal Experience by Roger Dowker for a detailed description of the commercial process, including when the various cut-off points are.

The trick to this appears to be the stuff legends are made of, and closely guarded by those who know. It's the matter of how much of the first condensate, or foreshots, to discard and how much of the middle cut to keep before discarding the last runnings, or feints.

For the various %'s at which to do the "cut", Donald advises to use a great hydrometer with 0.5% or greater calibrations for best results, and suggests ...

MashFirst DistillationSecond Distillation
Grainsto 18% (98 °C)85%-58% (80.5 °C - 92 °C)
Fruitto 25% (97.5 °C)85%-60% (80.5 °C - 91.5 °C)

When about 2/3 - 3/4 of the way through the middle run, and approaching these cut points, start collecting the spirits in smaller collection containers, and smell each of them seperately. The flavour will change from that of the neutral spirit, to more and more of the flavour coming through. This will intensify, but then start to become bitter. You need to work out when to make your "cut" during this period, but do so before it gets to the bitter stage. After making the cut, keep collecting (seperately) the feints up to about 92 °C, and add these to future runs.

For a reasonable whisky without the long term maturation try this : Repeat the whole exercise several times until you have enough of the low wines to fill your still. (Commercial distilleries get around this by using a smaller still for the low wines).

Load the still with the low wines and set it going. It's this re-cycling of the feints each time that does the magic, as they contain the higher alcohols (fusel oils), and esters.

You can now take the 5 litres, flavour it a little bit, put it in a small keg or flavour it with some oak essence. If kegging cut with water to around 40% or the angel's share will get too much. Don't charcoal filter or polish this spirit, as all the tasty bits you've just worked so hard to obtain will go too.

In order to get congeners, as opposed to a neutral profile it is important not to have a definitive reflux device in the steam path - enough refluxing will occur within the headroom, the "roof" of the still body, the lyne arm or equivalent. Make sure the still is only filled to about the three quarter mark.

As the weather becomes hotter and hotter in the southern hemisphere pot distillers put less wash in the body of the vessel thereby allowing more head for particulates of the solid variety to not be entrained [carried over] into the distillate. If you have variable control throttle back a bit.

Using a Reflux Still

The alcohol coming off a reflux still will be more distinctive / occur in steps. Rather than a gradual increase in temperature over the coarse of the run, it will get up to certain temperatures (near those listed above for pure fractions), then tend to sit there. The alcohol coming off will be of a fairly steady purity right through, only dropping off late towards the end. You'll probably finish a reflux run at a lower temperature (say 92-94 ° C) than a pot still (say 96 ° C.

For example, my 20L still takes about 1 hour to heat up, then once it gets to about 40 ° C, it then heats up pretty quick to 65-70 ° C. It will then sit there for around 5 minutes, and the first liquid (distillate) starts condensing. After about 5 mL of distillate have collected, the temperature then starts climbing again, up to 80-90 ° C.(Note that these temperatures aren't exactly as in the table above. The water & ethanol form an mixture that boils at a higher temperature - as shown in the graph way back in the Theory section). It will then sit there for the next 2.5-3 hours, and I collect the distillate at the rate of approx 1L/hour. (with my improved reflux still, it now sits steady on 78.2-78.4C for most of this period - eg 95% purity) Slowly towards the end of this period, the temperature slowly starts increasing up towards 90-94 ° C. By this stage, my hydrometer shows me that the alcohol is only about 40%, and I've usually had enough, so I then turn it off. Total time 4 hours. (with the new reflux still, I finish collecting at around 82C, as past there it deteriorates fast towards the rubbish - still 4 hours though)

Likewise, finish distilling at 92-94 ° C, as you've basically got all the easy ethanol, and you're starting to collect the higher ends, heavy in fusel oils (the wet cardboard smell).

Rob has the following advice running a reflux still : Ian Smiley's book "Making pure corn whiskey" http://www.magma.ca/~smiley/main.htm has very detailed instructions for using a reflux still or fractionating column for making whisky, by closely following recommended cut points (similar to those above); they can likewise be used for rums.

Using a Fractionating Still

The difference here is the need to really equilibriate the column at the start of the run, so that the methanol gets to accumulate at the top of the column, and to get all the packing in the column up to its equilibrium temperature so that it will work its best. This can take from 1-4 hours.

To get a fractionating still to work at its best also requires quite a high reflux ratio - returning 8-12 times back to the column vs that which is kept. To do this means knowing what the total rate is, then trimming the offtake valve to only take a portion of it. Do this by opening the valve fully and measuring how fast it is coming out, then closing down to only take what you should. Once you know this setting (say 1 drip per second), it will be the same for future runs.
If the wash is % alcohol, you have an W heating element, and you are collecting the distillate at mL/min
the distillate flowrate would be mL per minute if you were to reflux none of it, but you presently have a Reflux ratio of

Using the collection calculator back up the page, you know how much alcohol you have to collect, thus it is easy enough to work out how long its going to take. You may figure that its not worth waiting quite so long, just to gain a couple of 0.? % improvement in purity. Experiment to find a reflux ratio that still gives you a suitable purity, without having to wait forever.

I control my one only by adjusting the reflux ratio. It will happily sit between 78.2 C and 78.4 C for most of the run with a low reflux ratio, but towards the end, the reflux ratio will need increasing more and more to hold it there. As this happens, change the receiving container, and keep the tails seperate.

Rum from a Reflux Still

Make the wash from diluted molasses. Arroyo recommends to split up the fractions out of a reflux still, and then recombine them. The fractions are collected as per .. Mix the fractions together as ...

Cloudy Spirit

Sometimes your spirit may turn a bit cloudy when its been left by itself. This can be due to a couple of reasons ..
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