Difference between revisions of "Distillation -- Operating a Still"

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== Safety ==
 
== Safety ==
  
Distillation vapor path should not be pressurized. Avoid potential clogs in the system.
+
Distillation vapor path should not be pressurized. Avoid potential clogs in the system. Don't use thin 1/8" tubing. Any tube big enough for you to breath comfortably through it. Narrow parts of the system, are prone to excessive back-pressure.                                                                                                                                                                                                                 
  
Secondary distillations should avoid open flames.
+
Secondary distillations should avoid open flames. Even first distillations require caution. You can easily distill directly to 80% alcohol in the first distillation. I've had a spill from the receiving flask flow to the open flame and flare up. I put the fire with a towel.
 
+
Liquid condensates should be directed far from boiler. Avoid concentrated flammable liquids near a source of ignition. Consider using electric heat for the boiler.
Liquid condensates should be directed far from boiler. Avoid concentrated flammable liquids near a source of ignition.
 
  
 
=== The Methanol Myth ===
 
=== The Methanol Myth ===
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Distillation of alcoholic spirits has been practiced for at least 800 years. Whisky has been made in Scotland for at least 500 years. I'm sure the Scots of 500 years ago knew significantly less about biology and chemistry than we know today, yet this whole concern about blindness is a fairly recent myth. (I don't mean to single out the Scots. Scotland has a bad rap these days just because they talk funny and wear kilts, yet Scotland was a major center of philosophy and science in the 18th and 19th centuries.)
 
Distillation of alcoholic spirits has been practiced for at least 800 years. Whisky has been made in Scotland for at least 500 years. I'm sure the Scots of 500 years ago knew significantly less about biology and chemistry than we know today, yet this whole concern about blindness is a fairly recent myth. (I don't mean to single out the Scots. Scotland has a bad rap these days just because they talk funny and wear kilts, yet Scotland was a major center of philosophy and science in the 18th and 19th centuries.)
  
The reason methanol is also called "wood alcohol" has nothing to do with wood being fermented into alcohol. The term "wood alcohol" comes from the fact that wood already contains methanol which can be directly distilled from the wood. This is how it was discovered. Yeast does not ferment cellulose into methanol. If it were easy to make methanol we wouldn't have an energy problem. What little methanol that shows up in fermented beverages comes from natural enzymes that break down pectin into methanol. Fruits that are high in pectin also contain the enzyme which converts their pectin into methanol. There is nothing in the fermentation process that enhances this.
+
The reason methanol is also known as "wood alcohol" has nothing to do with wood or cellulose being fermented into methanol. The term "wood alcohol" comes from the fact that wood already contains methanol which can be directly distilled from the wood without fermentation. This is how methanol was discovered. Yeast does not ferment cellulose into methanol. If it were easy to ferment methanol from wood we wouldn't have an energy problem. What little methanol that shows up in fermented beverages comes from natural enzymes that break down pectin into methanol. Fruits that are high in pectin also contain the enzyme which converts their pectin into methanol. There is nothing in the fermentation process that enhances this. They are separate processes.
  
The origin of the myth that homemade liquor will blind or kill you comes from instances where unscrupulous or stupid people adulterated homemade liquor with industrial solvents such as methanol in order to boost its "kick". Sometimes people don't understand the difference between methanol and ethanol. This is still
+
The origin of the myth that homemade liquor will blind or kill you may come from instances where unscrupulous or stupid people adulterated homemade liquor with industrial solvents such as methanol in order to boost its "kick". Sometimes people don't understand the difference between methanol and ethanol and will confuse the two. This is still a big problem in India where people will sometimes use industrial methanol solvent as a cheap substitute for distilled ethanol.
  
 
=== byproducts ===
 
=== byproducts ===
  
The two biggest byproducts you will get in your liquor are acetone and acetic acid. Acetic acid is just vinegar and is relatively harmless; although even a little bit makes for a smelly, harsh drink. Acetone is less harmful than most people think. Most of it is easy to keep out of what you drink, but even if you left it in the worst you will get is a bad hangover. This description is actually a simplification. You will get a wide variety of Carboxylic acids and Ketones.
+
The two biggest byproducts you will get in your liquor are acetone and acetic acid. Acetic acid is just vinegar and is relatively harmless; although even a little bit makes for a smelly, harsh drink. Acetone is less harmful than most people believe. Most of it is easy to keep out of what you drink, but even if you left it in the worst you will get is a bad hangover. This description is a simplification. You will actually get a wide variety of Carboxylic acids and Ketones.
  
 
Note the boiling points of various components of a fermented mash:  
 
Note the boiling points of various components of a fermented mash:  
Line 35: Line 34:
 
*Water boiling point 100 °C
 
*Water boiling point 100 °C
 
*Acetic acid boiling point 118-119 °C
 
*Acetic acid boiling point 118-119 °C
Note that acetone and methanol boil quite a bit lower than ethanol. These will boil off first and will be the first to come out of the still.
+
Note that acetone and methanol boil quite a bit lower than ethanol. These will boil off first and will be the first to come out of the still. This is called the '''heads''' and is usually thrown away or recycled. Some warn you that you '''must''' throw these away or you could risk poisoning yourself. In a small still operation (say a 10 Liter reflux still) this is unlikely. I've saved and drank the heads pure with no ill effects, except mild regret. They don't taste nice. A large industrial still will produce a very pure concentration of acetone in the heads, so it would be unwise to repeat this stunt with a large still. Distilleries are a minor source of industrial acetone.
  
 
== Yields ==
 
== Yields ==
  
As a rule of thumb, expect an 16:1 yield of mash:50% alcohol. So, 16 liters of mash should yield 1 liter of 50% alcohol (100 proof).
+
As a rule of thumb, expect an 16:1 yield of mash:50% alcohol. So, 16 liters of mash should yield 1 liter of 50% alcohol by volume (100 proof).
 
<pre>
 
<pre>
 
16 : 1
 
16 : 1
 
</pre>
 
</pre>
That's a minimum to expect when first setting up a still. You are probably extracting only half the total alcohol available. With skill, careful distillation, and improved fermentation you can expect better yields.
+
That's a low estimate of what to expect when first setting up a still. At that yield you are probably extracting only half the total alcohol available (assuming a mash alcohol between 6% and 12%). You can expect better yields as your skills improve in fermentation and running the distillation process. With a 12% wine I can get 5:1 yield of around 40% alcohol with very little trouble.
  
 
== yeast ==
 
== yeast ==
Line 53: Line 52:
 
A note on '''worms''': when most people think of distilling they imagine a device with a long copper coil for a condenser. I do not use this form of still myself. A decent water jacket condenser is far superior to a worm. My main complaint about a work is that it's impossible to clean. As copper oxides build up inside the condenser they will effect the flavor of the fluid passing through it. A straight water jacket condenser is trivial to clean. I just run wads of paper through it with a rod. It's like cleaning a shotgun. I have no idea how you would clean a worm condenser.
 
A note on '''worms''': when most people think of distilling they imagine a device with a long copper coil for a condenser. I do not use this form of still myself. A decent water jacket condenser is far superior to a worm. My main complaint about a work is that it's impossible to clean. As copper oxides build up inside the condenser they will effect the flavor of the fluid passing through it. A straight water jacket condenser is trivial to clean. I just run wads of paper through it with a rod. It's like cleaning a shotgun. I have no idea how you would clean a worm condenser.
  
== hydrometer ==
+
== hydrometers (alcoholmeters) ==
  
Distilled spirits are measured in '''proof''' and '''%ABV''' (percentage of alcohol by volume). Proof is obsolete, but it is still popular in the United States, but legally, all alcohol is labeled in '''%ABV'''. Most manufacturers still include '''proof''' on their label because people expect it, but if you look you will always see '''%ABV'''. In the US '''proof''' is simply half a percent, so '''100 proof''' is '''50 %ABV''' (The United Kingdom used a different scale for "proof".). The '''%ABV''' scale is sometimes called a '''Tralles''' scale (not Tralle's, not Tralle, not Traille.).
+
Distilled spirits are measured in '''proof''' and '''%ABV''' (percentage of alcohol by volume). Proof is obsolete, but it is still popular on labels in the United States, but even in the US all alcohol must labeled in '''%ABV''' (proof is optional, but not required). Most manufacturers still include '''proof''' on their label because people expect it, but if you look you will always see '''%ABV'''. In the US '''proof''' is simply half a percent, so '''100 proof''' is '''50 %ABV''' (The United Kingdom used a different scale for "proof".). The '''%ABV''' scale is sometimes called a '''Tralles''' scale (not Tralle's, not Tralle, not Traille.).
  
Alcohol hydrometers for distilled spirits usually measure alcohol by volume. The scales usually read '''proof''' and '''Tralles'''.  They are referred to as '''Proof and Tralles''' hydrometers. Note that '''Tralles''' is frequently mispelled as '''Tralle's''', '''Tralle''', '''Traille'''. '''Tralles''' is the correct name as it is named after '''Johann George Tralles'''.
+
Alcohol hydrometers (alcoholmeters) for distilled spirits usually measure alcohol by volume. The scale usually reads both '''proof''' and '''Tralles''', so this type of hydrometer is referred to as a '''Proof and Tralles''' hydrometer. Note that '''Tralles''' is frequently misspelled as '''Tralle's''', '''Tralle''', '''Traille'''; in fact, I find that it is misspelled more often than now, but '''Tralles''' is the correct name because it is named after the man who invented it, '''Johann Georg Tralles'''.
  
Beer and wine hydrometers are used to measure properties of mash and wine '''before''' distillation. They are not used to measure '''proof''' or '''%ABV'''.
+
A Tralles hydrometer works based on the assumption that the liquid being measured is mostly water and alcohol. The volume of all the other components (the flavor and color) is considered to be insignificant in measuring the ratio of water and alcohol. A Tralles hydrometer cannot be used to measure alcohol in other liquids such as beer, wine, or mash. These liquids require their own special hydrometers calibrated to the properties of a mash '''before''' distillation. Using a Tralles hydrometer with these liquids would give wrong values.
  
 
== recipes ==
 
== recipes ==
Line 85: Line 84:
 
=== Simple Corn Whiskey ===
 
=== Simple Corn Whiskey ===
  
This is basically like '''Bread Rum''' but with the addition of a can of corn.
+
This is basically like '''Bread Rum''' but with the addition of a can of corn. This may seem strange, but it works very well.
  
 
*1 gallon of water
 
*1 gallon of water
Line 118: Line 117:
  
 
== misc ==
 
== misc ==
 +
 +
;ogee: a component of a '''pot still'''. It is a bubble-shaped chamber that connects the swan neck to the pot. It is a form a reflux column. It causes some of the distillate vapor to expand, condense, and fall back to the boiler to be distilled again.
  
 
;ranbiki: a form of Japanese still usually made of ceramic. Introduced to Japan by the Portuguese and Dutch in the late 1600's. Basically similar to an alembic still.
 
;ranbiki: a form of Japanese still usually made of ceramic. Introduced to Japan by the Portuguese and Dutch in the late 1600's. Basically similar to an alembic still.

Latest revision as of 12:24, 3 March 2015


Beware: these are very rough notes.

Notes on stills, making a still, distilling, how to distill, distillation of alcohol.

Distilling alcohol is as easy as making ice cream -- maybe easier.

How to make a still

Safety

Distillation vapor path should not be pressurized. Avoid potential clogs in the system. Don't use thin 1/8" tubing. Any tube big enough for you to breath comfortably through it. Narrow parts of the system, are prone to excessive back-pressure.

Secondary distillations should avoid open flames. Even first distillations require caution. You can easily distill directly to 80% alcohol in the first distillation. I've had a spill from the receiving flask flow to the open flame and flare up. I put the fire with a towel. Liquid condensates should be directed far from boiler. Avoid concentrated flammable liquids near a source of ignition. Consider using electric heat for the boiler.

The Methanol Myth

Distillation of alcoholic spirits has been practiced for at least 800 years. Whisky has been made in Scotland for at least 500 years. I'm sure the Scots of 500 years ago knew significantly less about biology and chemistry than we know today, yet this whole concern about blindness is a fairly recent myth. (I don't mean to single out the Scots. Scotland has a bad rap these days just because they talk funny and wear kilts, yet Scotland was a major center of philosophy and science in the 18th and 19th centuries.)

The reason methanol is also known as "wood alcohol" has nothing to do with wood or cellulose being fermented into methanol. The term "wood alcohol" comes from the fact that wood already contains methanol which can be directly distilled from the wood without fermentation. This is how methanol was discovered. Yeast does not ferment cellulose into methanol. If it were easy to ferment methanol from wood we wouldn't have an energy problem. What little methanol that shows up in fermented beverages comes from natural enzymes that break down pectin into methanol. Fruits that are high in pectin also contain the enzyme which converts their pectin into methanol. There is nothing in the fermentation process that enhances this. They are separate processes.

The origin of the myth that homemade liquor will blind or kill you may come from instances where unscrupulous or stupid people adulterated homemade liquor with industrial solvents such as methanol in order to boost its "kick". Sometimes people don't understand the difference between methanol and ethanol and will confuse the two. This is still a big problem in India where people will sometimes use industrial methanol solvent as a cheap substitute for distilled ethanol.

byproducts

The two biggest byproducts you will get in your liquor are acetone and acetic acid. Acetic acid is just vinegar and is relatively harmless; although even a little bit makes for a smelly, harsh drink. Acetone is less harmful than most people believe. Most of it is easy to keep out of what you drink, but even if you left it in the worst you will get is a bad hangover. This description is a simplification. You will actually get a wide variety of Carboxylic acids and Ketones.

Note the boiling points of various components of a fermented mash:

  • Acetone boiling point 56-57 °C (21 °C difference from ethanol)
  • Methanol boiling point 64.7 °C (14 °C difference from ethanol)
  • Ethanol boiling point 78.37 °C (22 °C difference from water)
  • Water boiling point 100 °C
  • Acetic acid boiling point 118-119 °C

Note that acetone and methanol boil quite a bit lower than ethanol. These will boil off first and will be the first to come out of the still. This is called the heads and is usually thrown away or recycled. Some warn you that you must throw these away or you could risk poisoning yourself. In a small still operation (say a 10 Liter reflux still) this is unlikely. I've saved and drank the heads pure with no ill effects, except mild regret. They don't taste nice. A large industrial still will produce a very pure concentration of acetone in the heads, so it would be unwise to repeat this stunt with a large still. Distilleries are a minor source of industrial acetone.

Yields

As a rule of thumb, expect an 16:1 yield of mash:50% alcohol. So, 16 liters of mash should yield 1 liter of 50% alcohol by volume (100 proof).

16 : 1

That's a low estimate of what to expect when first setting up a still. At that yield you are probably extracting only half the total alcohol available (assuming a mash alcohol between 6% and 12%). You can expect better yields as your skills improve in fermentation and running the distillation process. With a 12% wine I can get 5:1 yield of around 40% alcohol with very little trouble.

yeast

Saccharomyces cerevisiae

Condensers

A note on worms: when most people think of distilling they imagine a device with a long copper coil for a condenser. I do not use this form of still myself. A decent water jacket condenser is far superior to a worm. My main complaint about a work is that it's impossible to clean. As copper oxides build up inside the condenser they will effect the flavor of the fluid passing through it. A straight water jacket condenser is trivial to clean. I just run wads of paper through it with a rod. It's like cleaning a shotgun. I have no idea how you would clean a worm condenser.

hydrometers (alcoholmeters)

Distilled spirits are measured in proof and %ABV (percentage of alcohol by volume). Proof is obsolete, but it is still popular on labels in the United States, but even in the US all alcohol must labeled in %ABV (proof is optional, but not required). Most manufacturers still include proof on their label because people expect it, but if you look you will always see %ABV. In the US proof is simply half a percent, so 100 proof is 50 %ABV (The United Kingdom used a different scale for "proof".). The %ABV scale is sometimes called a Tralles scale (not Tralle's, not Tralle, not Traille.).

Alcohol hydrometers (alcoholmeters) for distilled spirits usually measure alcohol by volume. The scale usually reads both proof and Tralles, so this type of hydrometer is referred to as a Proof and Tralles hydrometer. Note that Tralles is frequently misspelled as Tralle's, Tralle, Traille; in fact, I find that it is misspelled more often than now, but Tralles is the correct name because it is named after the man who invented it, Johann Georg Tralles.

A Tralles hydrometer works based on the assumption that the liquid being measured is mostly water and alcohol. The volume of all the other components (the flavor and color) is considered to be insignificant in measuring the ratio of water and alcohol. A Tralles hydrometer cannot be used to measure alcohol in other liquids such as beer, wine, or mash. These liquids require their own special hydrometers calibrated to the properties of a mash before distillation. Using a Tralles hydrometer with these liquids would give wrong values.

recipes

Bread Rum

  • 1 gallon of water
  • 1 pound of sugar
  • 1 packet of yeast
  • 1 slice of wheat bread

Put the slice of bread in a blender and blend until you have fine bread crumbs. Add a few glasses of water. Add yeast and blend again to mix the yeast well. Let this sit while you prepare the rest. Add sugar to 1 gallon jug. Add hot water to cover sugar. Swirl this around until the sugar seems dissolved. Add cold water to almost fill the jug, but leave a little room for bread mash. Add the bread mash to the jug. Cover the opening of the jug with aluminum foil or an air-lock device. After a day the mixture will start to fizz and bubble like beer. Let this ferment for four days to a week or until the mixture seems to stop fizzing. Distill the mash.

Simple Corn Whiskey

This is basically like Bread Rum but with the addition of a can of corn. This may seem strange, but it works very well.

  • 1 gallon of water
  • 1 pound of sugar
  • 1 can of corn (12 ounces, cooked, unsalted)
  • 1 packet of yeast
  • 1 slice of wheat bread

Put the slice of bread in a blender and blend until you have fine bread crumbs. Add the can of corn to the bread and blend until smooth. Add yeast and blend again to mix the yeast well. Let this sit while you prepare the rest. Add sugar to 1 gallon jug. Add hot water to cover sugar. Swirl this around until the sugar seems dissolved. Add cold water to almost fill the jug, but leave a little room for the corn mash. Pour the corn mash into the jug. Cover the opening of the jug with aluminum foil or an air-lock device. After a day the mixture will start to fizz and bubble like beer. Let this ferment for four days to a week or until the mixture seems to stop fizzing. Distill the mash.

Blind Man's Bluff

Doctor Whoch

Don QED Rum

  • 1 gallon of water
  • 1 pound of sugar
  • 1 packet of yeast
  • 1 slice of bread

misc

ogee
a component of a pot still. It is a bubble-shaped chamber that connects the swan neck to the pot. It is a form a reflux column. It causes some of the distillate vapor to expand, condense, and fall back to the boiler to be distilled again.
ranbiki
a form of Japanese still usually made of ceramic. Introduced to Japan by the Portuguese and Dutch in the late 1600's. Basically similar to an alembic still.
alquitara
a Spanish and Portuguese style of pot still. It is a simple still somewhere between an alembic and a pot still.
poitín
an Irish liquor usually made with potatoes. Poitín means "little pot", as in a small pot still. Poitín had a notorious reputation and was usually made illegally.
pot still
the most common form of still. Pot stills are a descendant of alembic stills. Pot stills usually have a separate boiler and condenser.
alembic
one of the earliest forms of still. Often the condenser was part of the boiler.
continuous still
an industrial still in which mash can be added continuously without having to shut down the still (as opposed to a "batch" still).
retort
synonymous with alembic still.
fenny
cashew or coconut liquor from India.
reflux
this is a device that multiplies the effect of a still. It condenses the vapor stream and redirects the fluid back into the vapor where the heat from the vapor vaporizes the the fluid again. While the fluid may move backward it gains a little bit each time it is vaporized. Each time it gets a little bit stronger. The water keeps moving backwards and drips back into the boiler.
doubler
this is a primitive form of reflux found in moonshine stills.
thumper
synonymous with doubler.
condenser
a device to condense the alcohol vapor into a liquid. This is the most important part of any still.
slobber
this device may be synonymous with doubler, but may also be used as a trap to stop sludge boiling over from the boiler from getting into the condenser.
submarine still
this was a form of moonshine still. The name refers only to the construction and shape, which resembles a submarine. It is not functionally different than any other type of still.
worm
a type of condenser made from a long length of pipe coiled tightly to save space.
coil
synonymous with worm.

references

File:secondary fermentation compounds.pdf

File:Drop by Drop.pdf by Wolfgang Michel and Elke Werger-Klein from the Journal of the Japan Society of Medical History, Vol. 50 (2004), No.4, pp. 463-492.

books

Mountain Spirits by Joseph Earl Dabney. This is one of the best books to have for the history and lore of moonshining.

More Mountain Spirits by Joseph Earl Dabney. Equally as good as his first book.

The Home Distiller's Workbook - Your Guide to Making Moonshine, Whisky, Vodka, Rum, and So Much More! by Jeff King. This is probably the best practical book for a beginner to get.

Making Pure Corn Whiskey: A Professional Guide For Amateur And Micro Distillers by Ian Smiley. This is a more advanced book. It has lots of good information in a small space. My only complaint is that it tends to make the process of making whiskey sound harder than it has to be, but it is intended for a more advanced audience.

web sites

http://www.moonshineheritage.com

http://www.blueridgeinstitute.org/moonshine/

formulas

volume to gallons
US gallon liquid = ft³ * 7.4805
1 US gallon = 3.78541 Liters

Rules of thumb

1 gallon ~= 4 Liters