Fractional distillation

Transfer the high wine back into the boiler and add sufficient water to give a total volume of about 12 litres. Close the draw-off valve in the still-head, run cooling water through the condenser and switch on the boiler. Be present when it comes to the boil to reduce heat input if necessary. 11. Reflux for several hours to equilibrate column. Check temperature. Periodically draw off a few ml. of distilate and sniff it to detect presence of heads. Put aside for future use as fondue fuel or...

Water supply

It is worth mentioning that there is considerable resistance to the flow of water through a 16 ft length of 3 i6 tubing and you may find that friction alone will be insufficient to hold in place the plastic tubing leading from the water supply in the house. There is nothing worse than having the water line blow off in your absence and finding your workshop flooded when you return. So play it safe. One neat solution to this problem is to use the metal fitting and 1 4 o.d. high-density...

Collection rate

In simple distillation or in beer-stripping you collect everything which vaporizes from the boiler, but in fractional distillation you collect only about 10 of it. The reason for this is as follows The efficiency of a fractionating column in separating liquids of different boiling points is dependent upon two factors. One is the length of column and the type of column packing, i.e. its physical characteristics. The second is the reflux ratio, i.e. the way in which the column is used. The...

First stage beerstripping

Beer-stripping is not absolutely essential and theoretically it would be quite possible to fractionally distil the beer itself. However, beer-stripping has a number of advantages. The chief is that the alcohol is concentrated into a relatively small volume in a relatively short time and quite a few of the impurities eliminated. It would be extremely tedious to fractionally distil all that beer at 4 ml per minute (it would take about 8 days). Also, the yeast is left behind and does not interfere...

Cover

A transparent cover for the laundry tub can be made out of thick sheet plastic or plate glass. The plastic is easy to work with but suffers from the disadvantage that it bends up at the edges as the high humidity in the fermenter expands the underside of the sheet. For clarity in viewing and stability in operation plate glass about V4 thick is what you need, even though it is a bit difficult for an amateur to work with. So have your glass supplier cut it for you. A laundry tub usually has a...

Soldering

Before discussing the construction of the column and stillhead a word should be said about soldering. There are two solders in common usage the low temperature lead-free solder which melts at around 350 C. and silver solder which melts at about 1300 C. It is possible to manage with just the low temperature solder, but there are situations where a small joint needs to be made close to an adjacent one, or close to a larger one which needs a large flame, and in such situations there is a danger of...

Scale of operation

The first thing to think about is the scale at which you wish to operate. In pondering this weighty matter, take into consideration the following points. The cost of materials for building a still is almost independent of size. For example, in N. America at least, the most expensive item, the boiler, will be virtually the same price within the range 9 litres to 100 litres. Secondly, the smaller the equipment you use the more often you will have to use it in order to produce a given volume of...

Water quality

A word must be said about the quality of water used to dilute pure 96 percent alcohol to the 40 percent which is characteristic of most spirits. Unless the water is very soft, hardness will precipitate out when alcohol is added because the calcium and magnesium salts which constitute the hardness are less soluble in an alcohol-water mixture than they are in water alone. Depending upon the degree of hardness the effect will vary from a cloudiness to a white precipitate which falls to the bottom...

Drain

The drain outlet of a laundry tub is designed to take a tailpipe for connection to the house drain and does not match the sizes used for normal plumbing. But if you use a brass tailpipe you can, with a little ingenuity, connect to it a 3A-inch ball valve and a hose connector. You will then be able to transfer the beer to the still using a length of hose with a female connection at both ends (such as used with washing machines). Also, you can connect a length of garden hose for washing and...

Vodka

To make vodka, fractional distillation equipment along the lines of that discussed in a later chapter must be used. The strong (190 proof), pure alcohol so produced is diluted with water to 40 to give vodka. In sharp contrast to all other spirits, most vodka, particularly the vodka made in N. America, is made from pure alcohol, i.e. alcohol from which all the heads and tails have been removed. The US Bureau of Alcohol, Tobacco & Firearms (BATF) defines vodka as A neutral spirit so distilled...

Stirrer

We have tried everything from an impeller mounted through the bottom of the laundry tub to a vertical shaft through the glass cover driven by a small motor, and there is no doubt that by far the best method uses a submersible circulating pump such as used in an aquarium. Submerge the pump below the surface so that no air can enter it. Aerating the water is important for the well-being of fish but in fermenting it would simply make the yeast grow at an alarming rate. Fermentation is an anaerobic...

Whisky brandy rum etc

The distiller of these products uses a simple pot still or a pot still slightly modified to give a small amount of reflux (see next section). Such stills effect only a crude separation of the fermented liquor into heads, tails and a middle fraction. The skill in making a palatable whisky consists of a) fermenting the mash under a carefully controlled set of conditions to generate a particular mixture of organic compounds, followed by b) distilling the mixture and discarding a portion of the...

Gin

Gin is really nothing more than a special case of a flavoured vodka, the flavouring agent in this case being mainly juniper berries but also small amounts of other botanicals such as orris root, cardamom, coriander. Different distillers use different recipes, which accounts for their slightly different tastes. In a later section of the book a description will be given of the equipment and procedure involved in steam-distilling juniper berries and other herbs to produce a flavouring essence...

Yeast

There are two forms of active yeast the instant, dry, powdered type and the active, moist variety which comes in blocks. Either one sort or the other will be obtainable from the baking section of your local supermarket or perhaps from a delicatessen and it makes little difference which you use. The powdered yeast is about three times as active, pound for pound, as the moist yeast in block form, so work out which of the two sorts is the best buy. If there isn't a great deal of difference in...

Principles

Some of what needs to be said about the principles of distillation was covered in the chapter on beverages, and there was also some mention in the chapter dealing with the construction of a still. In both these places, the distinction was made between the comparatively simple pot stills used in the manufacture of whisky and the more elaborate still with fractionating column used to remove all the impurities and leave a pure alcohol, as in the manufacture of gin and vodka. The present chapter...

Economics

The next question is is it worth it Well, we have made 11 litres of vodka from 12.74 worth of sugar and yeast and 1.26 worth of electricity, so that works out at 1.27 per litre. Not bad. But how about all that equipment Let's assume a figure of 600 for its cost and see how long it would take to pay this off from the savings we realize on making our own vodka instead of buying it. If we produce and consume 1 litre of vodka per week it has cost us 1.27 against...

Boiling Point C

Chemicals of different volatility such as those in the table above have different vapour pressures, the most volatile with the lowest boiling point having the highest vapour pressure at any particular temperature. A liquid boils when its temperature is raised to the point where its vapour pressure equals atmospheric pressure. When a mixture of liquids of different boiling points is heated the vapour contains all the compounds which are in the liquid but is slightly richer in the more volatile...

Construction

In Figure 3. a still is shown which, because of its offset design, we refer to as the Mexican cactus. It consists of a 25 litre boiler surmounted by a 2V2 to 3 ft. length of IV4 copper tubing. This is the column. It will be packed with a suitable material (to be discussed later). At the top of the column is the stillhead where the vapours rising from the boiler are condensed to liquid and the liquid then split into two streams. The major stream, consisting of 90 of the condensed liquid, flows...

Steam distillation

Steam distillation requires the use of a simple pot still, and an example of such a still, improvised from a coffee pot, is shown in Figure 9 to illustrate the principle. Depending on how much steam distilling you are thinking of carrying out you may wish to devise and make a much larger and better one. One requirement is that it must have a large opening for introducing and removing the botanicals, these botanicals either being used loose or contained in a muslin bag for easy removal. A...

The packing

The packing inside a fractionating column is very important and many articles in the scientific literature are devoted exclusively to this topic. Everyone has his own ideas on what constitutes the ideal packing and the writer is no exception. Unlike scientific texts, however, cost is a consideration here. What is needed are pieces of glass, ceramic or metal which are inert to the liquid being refluxed and which have the following characteristics a) they should not pack tightly and should be of...

Power supply

The packed column which will be mounted above the boiler (see later) has only a limited capacity to allow vapours to rise up through the packing against the downward flow of condensed liquid so the boil-up rate must not be too great or the column will choke (flood). The 1500 or 3,000 watt heater supplied with these boilers is, in fact, unnecessarily large and we need to reduce this wattage to about 750 in some way. Several methods for doing this suggest themselves. One would be to buy a 750...

Headaches and hangovers

Headaches and hangovers are well-known consequences of overindulgence in alcohol, but what is far less well known is that these unpleasant side-effects are largely due to the impurities, the congeners, and not to the alcohol per se. This interesting fact will be confirmed by many people who habitually drink gin or vodka rather than pot-distilled spirits such as rye, bourbon, scotch, rum or even wine and beer. More objective proof that the congeners and not the alcohol are the bad actors can be...

Principles of steam distillation

Whereas ordinary distillation deals with the separation of miscible liquids, e.g. water, ethanol, methanol, etc., steam distillation deals with the separation of immiscible or partially miscible liquids, e.g. oil and water. When two immiscible liquids are heated, each exerts its own vapour pressure independently of the other. When the sum of the vapour pressures of the two liquids becomes equal to the atmospheric pressure, the two distil over together, and the temperature of distillation and...

Labour

It takes about 7 days from the time the fermentation starts to the time the collection of the pure alcohol is complete. During this period the amount of time involved in actually doing something with one's hands is probably no more than 3 or 4 hours. Periodically it is necessary to check a temperature or change a collection bottle but, to a large extent, the operation carries on quite happily by itself. It is not possible, therefore, to assign a cost to labour and we shall not attempt to do so...

Equipment

The production of pure alcohol by distillation is not particularly difficult in principle you simply have to make a batch of beer and then purify it. One cannot use a pot still however, or a moonshine still, or any of the strange little stills being written about and offered for sale on the Internet. This is because they do not incorporate the two essential requirements for high-purity fractional distillation. These two requirements are a) a packed column, and b) a split-stream stillhead. In...

Distillation what is it

To distil a liquid one simply brings it to the boil and condenses the vapour on a cold surface. To remove the hardness from water it is boiled in a kettle and the steam which is produced condensed against a cold surface to give a pure water free of minerals and all other types of impurity. The calci um and magnesium salts which constitute the hardness are non-volatile and remain behind in the kettle. Nature carries out her own distillation in the form of rain the sun evaporates water from the...

The condenser

The alcoholic vapours are condensed by means of cold water running through a coil of copper tubing inserted in the stillhead. To make this coil use 16 feet or so of 3 i6 flexible copper tubing.** Such tubing is not usually stocked in the plumbing section of a hardware store but can be found in the automotive supply section since it is used for fuel lines. Even Vg tubing can be found there if required, so don't be fobbed off by a salesman saying that W tubing is the smallest made. Make a hairpin...

Simple distillation

As mentioned before, the fermentation of sugars derived from grapes, barley, corn, potatoes, molasses, milk or any other source produces a wide variety of chemicals, the major one being ethyl alcohol (ethanol). Minor constituents will be methyl, propyl, butyl and amyl alcohols, aldehydes, ketones, esters, and a host of other organic compounds in small amounts. Analytical methods such as chromatography reveal that there are literally hundreds of compounds present after a fermentation. These...

Fermentation

Clean the fermenter and accessories with soapy water and rinse. 2. Close valve under fermenter and place a rubber stopper in drain hole. Install circulating pump and add 10 kg of sugar and the hydrometer. 3. Run in tap water. When water level is above the circulating pump start the pump, being careful to avoid any undissolved sugar crystals getting into the pump inlet. 4. Make up a yeast cream using 1 lb. of active baker's yeast in block form. Break into pieces and soak in a small volume of...

Costs Economics

What does it all cost you ask All that equipment and those elaborate procedures The answer is quite a lot, approaching 1000 in fact if you start from scratch. Is it worth it Well, that is a very individual decision and to help you decide, an estimate has been made of all the major costs involved, and also some of the minor ones. Prices vary from country to country of course, and it's always possible to make shortcuts, but we feel it's best to be realistic and not pretend that these things can...

Temperature measurement

A word must be said here about the accuracy of thermometers. A thermometer purchased from a scientific supply house should be accurate to 0.1 deg. C. but don't count on it. Thermometers purchased at a drugstore or a winemaker's supply store can be off by as much as 2 degrees. We recommend that you always check the accuracy of a thermometer by placing it in boiling water and recording the temperature. You may be lucky and find you have purchased one which reads 100 deg. C. but if it doesn't,...

The column

The fractionating column consists of a 21 z to 3 ft. length of 1V4 tubing. The rule of thumb is that the height of a column should be at least 15x its diameter, which would mean a column height of 19 minimum, but why not be generous and add a few more inches. The higher the column the better (within reason), because it provides a larger number of solid vapour interfaces up the length of the column and therefore more re-distillations. Two and a half to three feet is convenient but you won't wish...

Cooling water requirements

A number of people have expressed concern about the volume of cooling water required to condense the vapour from a 750 watt heater operating over many hours. It is not all that great, but if water is scarce or expensive where you live you will be interested in the following calculations. The calculations cannot be exact because there are many imponderables. For example, the temperature of the cooling water, the permitted rise of cooling water temperature, the desired drop in the temperature of...

Procedure

Those of you who are familiar with the making of beer and wine will find the fermentation of supermarket sugar with baker's yeast in a laundry tub a rather simple and crude procedure. Don't be disconcerted by this. All we are doing at this stage of gin- and vodka-making is producing the alcohol we need. Not being the final product, and not being intended for drinking, our concern is simply to make the alcohol as rapidly and as cheaply as possible. Taste is of no importance. The sophistication...

Support table

A fractionating still is rather tall and needs some support. Some people build their still close to a wall so that they can use brackets to support the column and the collection bottle. Another method is to make a table 30 high, put the boiler underneath and bring the column up through a hole in the tabletop. The hole should be large enough to accommodate both the column and the insulating sleeve around it. Use a spirit level to ensure that the column is upright. Not only does the tabletop...

Boiler

When it comes to amateur distilling there seems to be a burning desire on the part of the handyman to improvise a boiler out of some odd vessel which happens to be available, and no-one should be surprised to learn that everything from pressure cookers to beer kegs to milk churns to vacuum cleaner tanks have been adapted by ingenious do-it-yourself types _ for this purpose. However, we strongly recommend that you save yourselves a lot of time, trouble and expense by using an ordinary domestic...

The Question of Legality

This chapter is written specifically for those readers who live in countries where it is currently illegal for amateurs to make their own homemade spirits. This means almost all of us. It is also written for government officials, politicians, law enforcement agencies, the news media and any advocacy groups with an influence on public policy. The conflict between governments and moonshiners has been going on for centuries and the reasons are not hard to find. From the government point of view...

The Hatstand model

1 4 X 3 8' compression fitting When faced with the problem of how to condense a stream of vapour to liquid and then split the liquid stream into two parts, everyone has his own idea of how to do it better, easier, more cheaply and more beautifully than the Mexican cactus design shown above. We, too, have played around with dozens of different ideas, and the conclusion reached is that there isn't anything too much wrong with the Mexican cactus. It has a lot going for it. But, to demonstrate that...

The fermenter

Before discussing distillation we need to make the alcohol. Many of you who read this book will have been making beer or wine for years and will have all the know-how and equipment you need for fermenting sugar to a potable alcohol. There may be others who aren't quite as familiar with the process, but even for the beer and wine makers perhaps especially for the beer and wine makers it is necessary to explain that fermenting for alcohol production is a very different type of operation to...

Steam distillation practice

Most people who read this book will be interested in the steam distillation of plant material in order to isolate the essential oils contained in the leaves, needles, berries, etc. One could build a steam generator and conduct the steam through a bed of plant material contained in a kettle, which is the method used commercially, but a simpler system consists of a kettle containing water at the bottom and a grid just above the water holding the plant material. When the water is boiled the steam...

Thermometer adapter

In both stages of distillation it is necessary to know the temperature of the vapour stream inside the system in order to know what's going on, since temperature and composition are closely related, and the simplest method for introducing a thermometer would be to use a cork. This is the method we used for many years but it leaves much to be desired and there is a better method. Hot alcohol water vapour is very aggressive and corks rather quickly turn into a gnarled object closely resembling...

The alcoholwater azeotrope

Water is an important constituent of the fermentation broth and with a boiling point of 100 deg. C. lies intermediate between the least and the most volatile components of the mixture. It has one important difference from the other components, however, in that it forms an azeotrope with ethanol. An azeotrope is a mixture of two liquids with a boiling point lower than either constituent. In the case of ethanol and water the azeotrope occurs at a mixture of about 96** percent ethanol (v v) and 4...

Activated charcoal

Most amateur distillers are familiar with activated charcoal, using it to remove some of the more noxious substances present in their crude spirit. An ordinary pot still, the standard type of equipment used by amateurs, produces moonshine, and this contains some pretty unpleasant things, so activated charcoal remains the only hope of removing some of the worst of them and producing a palatable beverage. By contrast, the alcohol produced by the equipment described in this book should not require...

Material of construction

Glass is really the best material to use for making small-scale stills, being inert, clean and transparent. One can see exactly what is going on inside and it is aesthetically pleasing. For those fortunate enough to have access to a glassblower, either at a university or research institute, and are willing to pay the fairly high cost, the construction of a glass still will be described later. For the majority of people the choice will have to be metal and the only decision left to make is...

Latent heat of vaporization

In order to know how much pure alcohol can be produced per minute or per hour by a 750 watt immersion heater we first need to know the rate at which the alcohol in the boiler is being vaporized and condensed in the still-head, i.e. the boil-up rate. When we know this volume we take 10 percent of it. That is the amount we can draw off and put into our martinis. As discussed in the text, there are two methods of determining the rate of vaporization from the boiler by direct measurement and by...

Effect of pressure on boiling points

The boiling points of liquids quoted in reference books refer to the values measured at a standard atmospheric pressure of 760 mm mercury. As we all know, atmospheric pressure changes, varying considerably from day-to-day as weather patterns change and cold or warm fronts cross the region. Atmospheric pressure also changes with elevation. Not everyone lives at sea level under a stable air pressure of 760 mm Hg so the following table will allow you to interpret any temperature readings you might...

The glass still

The glass still shown in Figure 7 and described in the following paragraphs is essentially the same as the hatstand model discussed above, but there are one or two innovations which make it particularly pleasing. All dimensions are given so you can take it along to a glassblower and he will know exactly how to make it for you. The column and stillhead are made from 38 mm O.D. glass tubing, joined by means of a 34 45 drip-tip standard taper joint. A teflon sleeve is placed between the male and...

Introduction

Many books are available to amateurs on the methods and equipment involved in making beer and wine, and such books can be found in abundance in most bookstores and in beer- and wine-making supply stores. However, when it comes to the use of a small still to produce distilled spirits it is no use looking in bookstores. To find books on this subject it is necessary to search the Internet for independent publishers, but then we run into another problem. The books which are found on the Internet...

The Fractionating Still

Fractionating Still

The purification of the crude beer produced from sugar and yeast is a 2-stage process, or even three in certain cases. The first stage is known as beer stripping and, as the name implies, is just a rapid and fairly rough method for separating most of the alcohol from the beer and leaving behind most of the water and the yeast. The volume of liquid after this first stage, a liquid known as high wine, is less than one-quarter of that with which we started. So if we started with 50 litres of beer...

Fire and explosions

This may sound a bit melodramatic but when you are dealing with a procedure for the first time, and know that alcohol is inflammable, you may wonder. Let's take the explosion issue first. At no time, from beginning to end, is there any pressure in the equipment used for distillation. It is always open to the atmosphere. Fully open. Completely open. You will see that this is so when you look at the equipment diagrams later on and read the description of the procedures involved. So don't worry...

Poisoning oneself

The belief that there is some inherent danger in distilling one's own spirits is widespread and is reinforced whenever the news media report that a number of people have been taken ill, or even died, as a result of drinking homemade spirits. People associate homemade spirits with distillation, with moon-shining, but in fact there is no danger whatsoever in drinking home distilled spirits, or even moonshine properly made. The danger lies in buying liquor from a bootlegger because in order to...

Simple distillation The pot still

First let's take a look at the simplest situation the events taking place in a pot still when beer is distilled. The vapour is richer than the liquid in the most volatile constituents, i.e. the ones with the lowest boiling points such as acetone and methanol in the above table. When they distil over they are referred to as the heads. There is no clear-cut separation of the various compounds so the heads will still be coming over when the ethanol starts to appear. Similarly, before all the...

Attachment to boiler

At the base of the column there is the problem of joining a glass column to the 3A pipe nipple on the boiler and you will require the services of a machinist to solve this problem for you. Glass-to-metal joints are always tricky, so four different arrangements are shown in Figures 8 a , b , c and Ball amp socket joint Compression joint FIGURE 8. ALTERNATIVE ATTACHMENTS - GLASS COLUMN TO BOILER d . In the first case a a teflon O-ring makes the seal between the base of the column and a brass...

Summary

In terms of ease of manufacture, the production of pure alcohol is a science, not an art, and results therefore can be guaranteed if the proper equipment is used and the correct procedures followed. There are no subtleties involved such as quality of grapes or the type of yeast used. The starting material can be corn, potatoes, grapes, wheat, rice, milk, molasses in fact anything which contains a fermentable sugar. One hardly even needs to worry about hygiene just add large amounts of bakers'...

Amateur distillation

It is understandable why a government would wish to put a stop to smuggling and moonshining for commercial purposes, that is to say in order to sell the product and avoid the payment of taxes, but why would there be a complete ban on distillation by amateurs, on a small scale and for their own use And why, commercially, should a distilled spirit attract a higher tax per unit of alcohol At the risk of being tediously repetitious it is worth reminding ourselves again that distillation is one of...

Beer and wine

Alcoholic beverages can be divided into two broad categories according to whether or not there is a distillation stage following fermentation. Beer and wine fall into the non-distilled category whereas whisky, rum, brandy, gin, etc. have all been distilled. The latter are often referred to as spirits or hard liquor. Simple distillation permits the removal of some of the more noxious congeners by discarding some of the first liquid to distil over the heads and the last the tails . The middle...

Alcoholic Beverages

All alcoholic beverages are made by fermenting a sugar solution with yeast, a process which converts the sugar to carbon dioxide and ethyl alcohol. Usually one does not start with a pure sugar but with fruit juices for wine, the starch in grains for beer and whisky, the starch in grain or potatoes for vodka, molasses for rum, etc. Over the centuries trial and error have shown that a bewildering variety of sugar sources can be exploited in this manner, even such an unlikely substance as milk...

Immersion heater

The optimum temperature for fermentation if one is thinking of speed rather than flavour is about 33 C. Fermentation itself generates some heat but probably insufficient to maintain this temperature, particularly if the room is cool. An external heat source, therefore, should be provided and since only 100 watts or so are required an immersion heater such as used in an aquarium is ideal. If it does not contain its own thermostat, or if you use a different type of heater, an ordinary light...

Table of Contents

Alcoholic Beverages Sources of fermentable Beer amp Distillation what is it Simple distillation pot stills Whisky, brandy, rum, Fractional distillation 3. Health amp Headaches amp Fire amp explosions 4. The Question Of Fermenter Fractionating still The boiler The column The still-head Offset design Mexican cactus 39 Linear design An advanced glass still The flavouring still Principles Procedure 7. Distillation Principles Procedures Beer-stripping Fractional distillation Collection Yield of...

Helen Zajchowski

Making pure ethyl alcohol at home is a satisfying and profitable hobby for those who live in countries where it is legal to do so. Do-it-yourself types, who currently enjoy making beer or wine, find it particularly interesting because it is a logical extension of both these activities. There is the same fermentation stage where sugar is turned into alcohol but then, instead of drinking the brew, it is subjected to a very rigorous purification process. This process is fractional distillation, a...