The "reflux" Still
~ Amateur 'alcohol' distillation/manufacture basics 'Hooch' ~ (updated 29th June 2017)

Be advised: I am not a professional distiller but I am a person who is concerned with the illegal distillation of spirits taking place causing blindness and other problems. I decided to simply place this article on line to give a little guidance to the home brewer because, if you are selling spirits and you are unaware of the dangers of Methanol, being a part of the output process, then you become 'karmicly' responsible for the injuries caused to those to whom you may be giving or selling your product to.

Please therefore note:

This information is given here due to the fact that many people have become blind over time and suffer other illnesses due to their ignorance as to the inherent dangers in the distillation of spirits process if the temperature are not understood. Some have even 'passed away' from methanol poisoning. (Methanol attacks the optic nerve)

Thus this 'paper' containing information collated by me is to assist you and your family if you 'venture' into manufacturing any home 'brewed' alcohol.

Regrettably, many suppliers of 'home brew' Stills do NOT warn people of the dangers of methanol and other poisonous substances within the distillation process. This document is simply my 'effort' to assist you the beginner, but you need to make the effort to fully comprehend the process.

Managing and comprehending the temperature personally rather than simply relying on the manufacturers stated operational program is required. If your 'final product' when tested shows E.G. 80% pure alcohol, then it MEANS that 20% of the contents is something else. Possibly the 'heads or tails' of lower or higher temperature poisonous by-products shown below or even water dilution that also evaporated off whist distilling.

~ Home brewed 'Moon shine or rotgut' ~

'Moonshine' means 'silly in the head' and probable methanol contamination. 'Rotgut' means 'sick in the stomach' due to imbibing poisonous substances. All this also results in a poor quality taste.

Back yard distillation can be carried out by anyone, and if you wish to personally imbibe what you have made is one thing, but when you give it or sell it to others and cause them to suffer somewhere down the road maybe years ahead, then there is a 'karmic' comeback.

One thing is for sure, if your distillation process requires you to 'boil' the 'whole' mixture through ignorance or from using uncontrollable heating, then you are evaporating the entire contents and contaminating the end product because the 'Still' reflux column will not separate out all the vapours. This can only be 'done' satisfactorily using a controlled temperature process.

Controlled temperature requires an adjustable temperature regulator as well as an adjustable heat. If you are using a 'fire' to boil the 'stuff' then you cannot control the heat and neither can any regulator controller.

If you do not have access to electricity that enables the use of a thermostat regulator, then your best option is to use 'gas' because you can control the heat very easily and rely on a thermometer. NOTE: If using gas then the liquid collection container must have a longer tube so that no liquid or vapour gets near the gas flame causing fire.

These pages are written by me simply to assist you to make a good quality 'home brew' and NOT simply rely on the advertising 'spiel' put out by home brew 'Still' manufacturers or others. You need to become personally responsible for what you give away to friends or what you sell to others.

The pure alcohol named 'ethanol' that  you seek within the sugar-yeast-water mix (brew) you make, evaporates out of the 'brew' at a temperature given below:  (Ethanol 79C = 175F) - however, as you are heating UP the brew at the start, the poisonous methanol that evaporates at the lower temperature (65 C = 150F) will start to vaporise FIRST.

What does this mean for you? It means that between the methanol vaporisation temp of 65C and the vaporisation ethanol temp of 79C, there is a SAFE temperature difference of 12 degrees C.

What I am saying is, that if you keep the brew temperature between 65C to below 75C in the initial stages, you will ONLY be vaporising the poisonous methanol and not losing any ethanol at the same time.

So keep the temperature of the 'brew' below 75C until all the liquefied methanol stops flowing from the 'still' - once it has fully stopped, then you must pour the liquid methanol collected down the sink hole and wash out the collection bowl before turning UP the 'heat' that will evaporate the ethanol when the brew temperature gets to above 79C. (Sea lever temperature)

If you control the heat at the beginning of the process to 75 C, a point where ONLY methanol is dripping out of the pipe into the receptor, then a purer product is obtained and you are not endangering the end user.

Note: Some distillation units being marketed which use about 20 L of 'brew' state that if you remove the first 50 ml that it will only be the Methanol, and after that, all else will be methanol free. This may not be the case, because it is giving you a 'fixed' volume. Better to keep collecting everything exiting the brew whilst the temperature is kept below 75C because, once it stops flowing, then you KNOW that ALL the Methanol is extracted.

Added note. Methanol must not get onto your skin as it enters the body and over time causes problems.

You will note from the 'tables' below that there are other poisonous substances (propanol) that start to vaporise at 82 degrees C, so the 'margin' of error is only 3 degrees C. It is important to NOT permit the temperature at the outlet of the still to rise above 81 degree C. (Sea level) If you do, then your distillate may become contaminated. 

The 'four' heads and tails in RED * below are all poisonous substances, however the 'tails' may not harm you due to being very small amounts, but which will cause a bad taste and smell. PLEASE DO YOUR OWN HOMEWORK - this is but to assist.

Sea level distillate temperature needed to vaporise:

(Heads) Methanol* : 65 C = 150F (approx )

Ethanol - 79C = 175F

(Tails) 2 Propanol* : 82C = 180F
1 Propanol* : 97.2C = 207F
3 methyl 1 Butanol* : 99.5C = 211F

Water - 100C = 212F

NOTE - Much of the below information is simply collated by me from other resources.

There is also a better informative link at the end on page 8

Distillation is a process in which vapour mixtures of six or more substances are separated into their individual components of desired purity by the application of heat. Distillation is based on the fact that components in a mixture of different liquids have different boiling points, thus the vapours can be separated.

Separation of components from a liquid mixture via distillation depends on the relative volatility of the individual components. This "difference" in "boiling points" enables separation by heating. Distillation columns are designed to achieve this separation efficiently.

The 'bubble-point' is the temperature at which a liquid starts to boil. The 'dew-point' is the temperature at which a vapour starts to condense. The 'Relative volatility' is the measure of the differences in volatility between substances, and hence the difference in their boiling points.

A liquid is said to ‘boil’ when its vapour pressure equals the surrounding atmospheric pressure. The 'ease' with which a liquid boils depends on its volatility. Liquids with high volatility will boil at lower temperatures. Rate of distillation/separation is dependant upon spirit evaporation.

Higher altitudes with less "relative" atmospheric pressure will induce any liquid to boil at a lower temperature. Distillation separation occurs because of the differences in the volatility of the components in the liquid mixture. (Difference in boiling/evaporation temperature). Therefore, when 'a' vapour is cooled and condensed, the condensate will contain more volatile components than the original mixture which will still contain the less volatile material.

Distillation columns or "towers" are designed to achieve this separation efficiently. A "wide" bodied column with "slow" vapour movement is best, as vapour pressure speed through a too narrow column can "carry-over" unwanted "precipitation" particles in suspension and its flow can be restricted more easily, thus slowing the process.

Heating a Still involves working with steam, electricity or open flame, and as explosive vapors are being formed you must take extreme care to prevent fire or explosion that will occur if spirit vapour is ignited by a naked flame.

Alcohol is a solvent formed by the fermentation of various products that are made into a "mash" that is "distilled" after 5 -10 days to draw off its pure spirits, being Ethyl alcohol (Ethanol.) The object of the distillation is to end up with a 190 "high proof" spirit that is 95% pure.

During a fermentation process there is the possibility of other "ols" being manufactured which are harmful to the biological body that need to be either distilled off first due to their 'lower' evaporating temperature, i.e. Methanol, or the 'higher' temperature 'tails' need to be left in the "Pot mash" by ensuring that they are not distilled off as their evaporative temperatures are higher than the Ethanol alcohol.

Beverages such as beers & wines that are not "distillates" do contain a percentage of "poisonous" substances that cause hangovers, blindness or death. Let it be known that any alcohol be it pure or otherwise is poisonous and can be fatal if taken too liberally.

The "beer" mash you start with might be simple (sugar, water, yeast), but after fermentation, the 'beer' contains many ingredients. It’s also important to recognize that some of these compounds have boiling points quite close to the Ethyl alcohol you are trying to distill off.

That means you will have to be careful about controlling the column temperatures to make sure that you collect only pure spirits. Some of them "spoil" the taste of the final product. A well designed Reflux Still is by far the best separator, and it will enable you to produce a much purer spirit than a Pot Still.

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Boiling a "mash" in a Pot Still does separate out alcohols, but unless you are fully aware of the 'why & what' etc, and repeat the process a few times you will end up with a lot of impurities, and it is thus that the Reflux Still is the "purer" way to go. In this type of "separator" you also need to know the temperature control requirements in order to "withdraw" the purest Ethyl alcohol that is the "base" of any alcoholic beverage.

The "amateur" needs to take the "pot luck" out of his "Still" by seeing what is taking place as its "energy" does "overspill." For there are "combustibles" to which man's "biology" cannot relate, and these must be removed by the "fire & water" grate/gate.

The "essence" of distillation is control over the gases formed as through the Still they "stroll." These gases one can regulate and separate as long as with "understanding" we "relate." So "temperature control" is the only way "uphill" as we "reflux" by "barring" the "exit" gate "play" of the Still by "coldness" until the correct temperature we reach for each gas that we would "leech."

Outer "cladding" is the way to go, so that all heat created is used and contained and fuel bills do not "overflow," and more easily can we control the "gas" outflow. If you clad the Still the inner temperature is easier to control, as is the "exhaust" particulate that needs not to "boil."

Let the condenser have its own separate regulated cooling water supply.
Let the "lower" Still cooling point have its own regulated water supply gate.
Let the "top" Still column "head" have its own regulated water supply gate.

Let the "cooking pot" have a temperature gauge.
Let the "lower" Still cooling point have a temperature gauge.
Let the Still column "head" have a temperature gauge.

This way the "column" of gas can be "minutely" regulated for "each" gas to be extracted, and minimal heating fuel is used as the "pot" brew is "started" at a Methanol inducing temperature of 70C and later maintained at an approximate 81C for Ethanol extraction.

The column "head" can also then be regulated "cool" as the "pot" content does heat up, and the 'gas' formed does "spool" up and down the column between the two column tower "water" temperature regulated points. As it "spools" or "refluxes" it "purifies" itself.

Once the initial gas flowing between these two points is "stabilised" at a required temperature, say lower 70C upper 62C, then the top column water supply is reduced to "permit" the top temperature to rise to 68C. This allows any Methanol to vacate the system and be condensed. But it does not permit any Ethanol to escape.

Once any Methanol condensate stops flowing then replace with a clean collection container marked "Ethanol" and raise the Still temperature slightly to commence distilling off the Ethanol. The lower column temperature can be maintained @ 80C and the upper @ 77C initially by regulating the water flow in the column as well as the heat applied. This will "permit" refluxing to take place between these two points as the column warms up.

After a few minutes begin to reduce the upper coolant water supply and permit the upper temperature to rise to 78.5C and the Ethanol will flow out into the condenser. The "speed" of the distillation outflow will depend on the amount of heat source given, but the column temperature needs to be kept within the lower 78.5C  & upper 81C limits by regulating the coolant water flow and heat input. This ensures that "higher" temperature evaporants such as Propanol stay condensed in the Still "pot" with the water.

Once the Ethanol condensate exiting the condenser slows down then halt the distillation process. Shut down the heat source and "open" the valve to "atmosphere" to avoid a vacuum forming as the unit cools, or the system could be damaged by atmospheric pressure collapsing the container.

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"Refluxing" in the distillation "context" means: Cooling the top column gas water coolant "gate" to the "point" whereby the gas condenses again prior to exit-ing the "tower" and "falls" back down the Still column to be reheated and thus it "cycles" or "refluxes" up and down and purifies itself. If the final product has been properly "separated" by "true" distillation then it will not require "additional" filtration by other means. This is done by passing the final product through activated carbon.

The column has plates or packing internally which are used to enhance component separation. Packings are passive devices that are designed to increase the interfacial area for vapour-liquid contact. The vapour cools and condenses on the packing, and not only causes some vapour to condense, but the condensed liquid is also made to evaporate by the rising warmer vapour, and in this process the product is refined as it fluxes between a liquid and vapour state, and also ensures a good distillate separation.

The "Pot" Stills of "old" do not separate contaminants from the alcohol, and thus it is imperative to know all the facts before using one to manufacture any product that may be contaminated. The "Reflux" Still design given here is more easily controllable and thus can produce the purest of spirits.

Distillation for the amateur is by "Batch," whereas the commercial operator would use a "continuous feed" process. The usual "home" batch quantity would be between a 10 to 30 liter "mash" that would render up between 1 to 5 liters of 95% pure Ethyl alcohol. This is then diluted approx 1 part to 3 parts of water to make up alcoholic beverages or herbal medicines of 40-25% alcohol content.

** Note, the "boiling/gas" point of Methanol, Ethanol etc given is at sea level with standard barometric pressure. Lower "evaporation" temperatures take place as you rise up to higher altitudes, and this needs be taken into account when living or 'distilling' at from 3,000 to 10,000 foot altitudes.

E.g. Propanol & other 'solvents' that gas at 82.4 or higher temperatures would be distilling off at a much lower temperature at high altitudes and thus contaminating your Ethanol. Equally, the Ethanol would also be "flowing out" at a much lower temperature and could be 'lost' whilst removing the Methanol unless the correct temperature/boiling point for the given altitude was known.

A big fear for some distillers is that they are risking poisoning themselves with Methanol, a toxin that can cause blindness. Methanol is formed when fermenting beverages high in pectins - e.g. grapes and berries and 'other' stock. If formed, it can be easily discarded with the "heads" collected first during distillation by using the correct temperature separation.

Starting with a grain or sugar based batch in a clean "crucible" with a yeast culture will result in minimal or no Methanol being formed. This article is for the many who use 'strange' raw materials to blindly 'concoct' beverages, and it is hoped that they will be more enlightened as to the inherent dangers and the correct way to distil in order to aid themselves and others. Do your own 'further' research. This is but a "beginners" course.

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Basics for fermentation

The Fermentation container. Preferably of a 40 Liter size if it is to contain 30 liters of mash/liquid having a wide "top" that enables the forming CO2 to escape the brew. The "lock" contains a water trap that allows the venting of carbon dioxide, but prevents the fermentation coming into contact with air (Oxygen, that counteracts production).

During fermentation the yeast consumes the sugar, leaving two by-products, alcohol and carbon dioxide. The carbon dioxide flows out through the fermentation lock and the alcohol remains in the mash. So that the yeast is able to last as long as possible, it must be given optimal conditions.

The fermentation process adds heat of about 5°C or more with larger quantities. If the temperature falls below 18°C fermentation will stop until the temperature rises once more. A bigger fermentation batch in a container of 100 or 200 liters ferments more rapidly than a smaller brew.

Clear mash must not stand on its lees for more than 3 weeks. It should be removed from the lees before the lees cause souring or oxidization. If this happens the oxygen in the air will oxidize the alcohol to acetic acid. During fermentation the carbon dioxide protects the mash from coming in contact with oxygen that would negate the fermentation process.

However, lees may be kept for many months as long as the fomenter has an airlock and it is not opened thus keeping oxygen out.

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The Hydrometer indicates when fermentation has ceased in the mash. When the instrument shows (spec. gravity 980-990) the fermentation is complete.

Fermentation usually starts at (spec. gravity 1080) or higher. Allow the hydrometer to float freely and read it off from the surface of the liquid. To find the alcohol percentage by volume, you need the difference between the starting and final readings, then divide by 7.75 or multiply by 0.129.

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Once the fermentation is complete, with the sg. below 1000, then a Siphon is used for transferring the finished clear liquid to another fermentation container for about 4 days. The yeast deposit is left behind in the fermentation vessel. This allows further settling and the liquid becomes clear. This 'clear' is then again Siphoned off into the Still.

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An Alcometer measures the alcoholic strength of the distillate. It functions in mixtures of alcohol and water and is graded from 0-100%.

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Temperature conversion

F = C multiplied by 9, and then divided by 5, and then add 32.
(C x 9 ÷ 5) + 32 = F
C = F minus 32, then divided by 9, then multiplied by 5.
(F - 32)  x 5 ÷ 9  = C

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Ingredients are of many "sources," but the basic Sugar/water/yeast mixes can be obtained from suppliers who have stocks of "high yield" Turbo yeast.

20 liters of mash needs approx 5 kg sugar
30 liters of mash needs approx 8 kg sugar

Baker's yeast and ordinary Turbo yeast cannot ferment out more than 14% alcohol. Only high alcohol-tolerant yeast can manage this, but takes longer and liquid temperature may not go over 26C.

Dissolve the sugar in warm water, and then fill up with cold water to give a volume of 20 or 30 Liters and a temperature of 20C. The sugar must be completely dissolved for the yeast to convert all the sugar into alcohol (called fermentation). Using 8-kg sugar you end up with a liquid of approx. 20% alcohol. The crystal clear mash is then drawn off and later distilled.

Providing you keep the liquid temperature below 30°C all the way through fermentation (25°C for very high alcohol) you will not kill the yeast. This is easy with volumes up to 30 Liters.

It is not so easy to keep the liquid temperature below 30°C when fermenting larger volumes and you need to keep the heat generation down, or cool the brew after about 10 hours into the fermentation. At 25°C fermentation of 25 L will take about 7 days. To keep down production of volatiles, a maximum liquid fermentation temperature of 25°C is recommended. 20 - 22 degree C is the best.

All liqueurs can be made from the finished product by either adding essences, or by adding fruit that is placed in the 'neat' alcohol for a couple of weeks, and strained out before 'reducing' the alcohol content to its drinkable levels of 25% - 40% by the addition of water.

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~ Methanol & its toxicity ~

Methanol is carbinol is wood spirit is wood alcohol. Methanol itself may cause inebriation but by itself in almost completely non-toxic. The Methanol is metabolized by alcohol dehydrogenase to formaldehyde and then to formic acid. Clinical findings correlate better with formic acid levels than with Methanol levels.

It is these two metabolites that cause toxicity, with formic acid being more responsible. It is the formic acid that causes the profound metabolic acidosis that is typical of Methanol poisoning. The overall mortality of Methanol poisoning is approximately 20% and among survivors the rate of permanent visual impairment is 20-25%.

Poisoning with Methanol may be accidental or intentional. There have been epidemics of Methanol toxicity in cases where illicit whiskey has been sold to large populations or when the less expensive Methanol was substituted for Ethanol in drinks.

Poisoning may occur from ingestion, inhalation or skin absorption. Symptoms include anorexia, severe abdominal pain, vomiting, diarrhea, increased transaminases or increased amylase. Early visual disturbances are the classic findings that are associated with Methanol intoxication and include decreased vision or blurred vision.

Other complications of severe Methanol intoxication include coma, seizures, blindness, oliguric renal failure, cardiac failure, and pulmonary edema. Death may be rapid or may occur several hours after coma. Death is associated with inspiratory apnea, terminal opisthotonos and convulsions. Fatal dose 100ml.

Ethanol is used to decrease the metabolism of Methanol. Alcohol dehydrogenase acts within the liver to break down both Ethanol and Methanol, and is the rate limiting step in the metabolism of both these alcohols. The enzyme, alcohol dehydrogenase, has a greater affinity for Ethanol than it does for Methanol. Therefore, in the presence of Ethanol, the metabolism of Methanol to its toxic metabolites is greatly slowed.

If there is a high clinical suspicion that a patient has ingested Methanol it is appropriate to begin an Ethanol drip while awaiting blood levels of Methanol. Ethanol drips are also indicated if the blood Methanol level returns and is 20 mg/dl or above. The target Ethanol level is 100-150 mg/dl since this is the level that will saturate alcohol dehydrogenase.

Methanol manufacture is a complex, high-pressure process in which very large scale production of engine fuel is produced via gasification of biomass, and can not be adapted for small scale operations.

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Properties of Ethanol & its toxicity

Ethanol is a monohydric primary alcohol. It boils at 78.5° C. It is miscible (i.e., mixes without separation) with water in all proportions and is separated from water only with difficulty; Ethanol that is completely free of water is called absolute Ethanol. Ethanol forms a constant-boiling mixture, or azeotrope, with water that contains 95% Ethanol and 5% water and that boils at 78.15° C; since the boiling point of this binary azeotrope is below that of pure Ethanol, absolute Ethanol cannot be obtained by simple distillation.

New technologies allow for the production of Ethanol from agricultural by-products such as corn stover, bagasse, yard and wood waste, sugar cane etc. And are used as the source of biomass substrate. Both Methanol and Ethanol are solvents that can be used in combustion turbines. Newspaper produces approx 100 gallons of Ethanol per ton.

Clinical Effects of Ethanol: The effects of moderate alcohol consumption is well known to most people. Patients present with dis-coordination, slurred speech, and later CNS depression. Patients may present with tachycardia, sweating, and flushing from Ethanol induced vasodilatation. Patients may also have mydriasis, dysarthria, incoordination, altered mental status, and nystagmus. At high doses Ethanol is a general CNS depressant.

The most important aspect of the management is recognition that the patient has been exposed to a toxic alcohol. Unless the amount of Ethanol or other alcohol is large and very recent there is very little indication for gastric lavage as the alcohols are well absorbed from the gut. Alcohol is broken down in the liver by alcohol dehydrogenase.

Concern should arise in those patients that present after having ingested extremely large amounts of Ethanol over a very brief period of time as Ethanol levels above .45 % can cause death from respiratory paralysis. Levels below this can cause hypothermia and loss of the normal protective airway reflexes. Infants and toddlers that ingest alcohol have a different course than do adults.

Medically, Ethanol is a soporific, i.e., sleep-producing; although it is less toxic than the other alcohols, death usually occurs if the concentration of Ethanol in the bloodstream exceeds about 5%. Behavioural changes, impairment of vision, or unconsciousness occur at lower concentrations. With levels as low as 50-100 mg/dl children can present with coma, hypothermia, and hypoglycaemia.

Patients with Ethanol intoxication may have an osmolar gap but do not usually have a marked metabolic acidosis or anion gap unless they have co-ingested some other substance or have ingested a truly toxic amount of Ethanol in which case they may be hypotensive and near apneic which would account for an acidosis. As with all altered mental status patients a glucose should be checked and if it seems indicated narcan and thiamine can be given.

Management: As with any patient presenting with an altered mental status and altered vital signs, attention must be paid to the ABC's. An odour of alcohol can be misleading in some cases as the patient may have co-ingested other more serious toxins or may have ingested significant amounts of an alcohol that does not smell.

All patients with altered consciousness and a smell of alcohol should be first assumed to have some other more serious condition, be a toxin or a physical injury. If there is a possibility of a large and recent alcohol ingestion, or any concern that there is a co-ingestion then it is reasonable to give charcoal after the airway has been secured. Glucose and thiamine are indicated in these patients. An Ethanol level should be sent early to help verify a suspicion of Ethanol intoxication.

Should the patient appear with coma and unstable vital signs or have known liver disease it may be reasonable to dialyse the patient as this can quickly and safely eliminated the Ethanol. This is only rarely indicated.

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Another source of distillation information is found at:

https://podilatokafe.files.wordpress.com/2014/01/545-pg-home-distillation-of-alcohol.pdf

Ends

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