16.3.

The 18th amendment to the United States Constitution prohibited "the manufacture, sale, or transportation of intoxicating liquors within, the importation thereof into, or the exportation thereof from the United States." The law was so popular that it was repealed thirteen years later. The current law in the United States allows each adult to brew up to 100 gallons of beer or wine for her own personal use and a home-brewing industry has grown up to service hobbyists. It remains absolutely illegal, however, to distill spirits without a government permit. Boot-leggers are enthusiastically hunted down by law enforcement officers who, like the tenth-century painter, want to keep a lid on the spread of spirits.

Still, Part 19.901 of the Code of Federal Regulations "implements 26 U.S.C. 5181, which authorizes the establishment of distilled spirits plants solely for producing, processing and storing, and using or distributing distilled spirits to be used exclusively for fuel use." To establish such a plant requires a simple alcohol fuel producer's permit, form 5110.74, which may be ordered from the Bureau of Alcohol, Tobacco, and Firearms.[1] There is no fee for the permit and no tax is levied on alcohol used as fuel. Do not imagine that such a permit allows you to drink your spirits. If you are going to break the law anyway, such a permit is of no use to you. But if you are driven by curiosity to experience first-hand one of the most marvelous, literally spiritual substances in all of chemistry, this "liquid, which when set on fire and while still flaming leaves the material [underneath] unburnt," such an easily-acquired permit allows you to do so without getting into hot water with the Feds.

Figure 16-6. The PVC Still

Of course, you will need a still and, there being no home-distillery market, you will have to either buy a still intended for laboratory use or build one yourself. Fortunately a still is not a particularly complicated piece of apparatus. I will tell you how to build one from an Erlenmeyer flask, a rubber stopper, and some common plumbing supplies. The complete still is shown in Figure 16-6(L) and the pot is detailed in Figure 16-6(R). Part (a) is a rubber stopper sized to fit the 500 mL Erlenmeyer flask, part (b). The stopper should have a hole drilled in it, 5/8 inch in diameter. Erlenmeyer flasks are not expensive and you can get one with a stopper from one of the suppliers listed in Appendix D. A flask weight will help prevent the still from tipping over. The one shown is constructed from four 3-inch sections of half-inch copper tubing, parts (c), and four elbows, parts (d), available from a plumbing supply. Fill the tubing with lead or steel shot before gluing it together with epoxy cement. The weight fits over the neck of the Erlenmeyer flask, which sits atop a hot-plate.

Figure 16-7. Details of the Column and Condenser

The column, detailed in Figure 16-7(L), is constructed from two 9-inch sections of half-inch CPVC tubing, parts (e), a common meat thermometer, part (f), two half-inch elbows, parts (g), and a section of tubing, part (h), long enough to accommodate the thermometer; the one shown is 4 inches long. Be sure to use CPVC tubing—the kind intended for plumbing hot water. Drill a hole in one of the elbows to make a tight fit with the probe of the meat thermometer. Use cement specifically designed for CPVC to glue the column together.

Any convenient container will serve as the receiver, part (i). The one shown in the figure is a 20-ounce soft drink bottle. The condenser, part (j), consists of the bottom of a 2-liter soft drink bottle filled with crushed ice. Commercial condensers are air-cooled or water-cooled, but the one shown works admirably without increasing the cost or complexity of the still.

You need a source of heat strong enough to boil water but not so intense as to crack the Erlenmeyer flask. Laboratories are equipped with hot-plates designed for exactly this purpose. Alternatively, there are many varieties of consumer appliances such as hot-plates, coffee makers, and crock pots which could be made to serve. Avoid anything whose heating elements visibly glow, as it may cause the glass to crack. It is a good idea to keep a leather work glove on one hand during the distillation so that you may quickly remove the still from the hot-plate if the temperature rises too quickly.

To operate the still, fill the Erlenmeyer flask with 400 mL of mead, wine, or beer. Add a couple of "boiling chips," small pieces of glass or silica, to prevent the still from boiling over. Slip the flask weight over the flask and insert the rubber stopper and column into the flask. Turn on the hot-plate, gradually turning up the power until the solution in the flask comes to a boil. Place the receiver into the condenser, fill the condenser with crushed ice, and slip the free end of the still into the receiver. The free end of the column should go all the way to the bottom of the receiver.

You are about to learn the truth of the old saw, "a watched pot never boils." You will watch the thermometer for some time with no change in its temperature. The temperature will begin to rise only when hot vapor makes it up the column to the head, the elbow where the thermometer lives. Do not get impatient—if you turn up the heat too quickly, the head temperature will be too high and your distillation will be spoiled. Eventually, the head temperature will rise and "steam" will exit the column into the receiver, where it will condense. Because the boiling point of ethanol is lower than that of water, your goal from this point on is to maintain the head temperature at the lowest possible value while still collecting liquid in the receiver. The boiling point of ethanol is 78C (172F); if you can keep the head temperature at or below 83C (181F) you will get reasonable separation of ethanol from water. If the head temperature gets a little too high, reduce the power to the hot-plate. If it is way too high, use your gloved hand to remove the still from the hot-plate and allow it too cool for a minute or so. After a while you will get into a "zone," in which the head temperature remains constant and liquid accumulates in the receiver. At some point you may wonder whether anything is coming out of the column; simply remove the receiver and cautiously feel the end of the column with your non-gloved hand. If it is hot, you are still collecting alcohol. Eventually you will find that you cannot continue collecting alcohol without increasing the head temperature. You will have collected most of your alcohol in the receiver and the pot will contain mostly boiling water and yeast carcasses. You may now turn off the hot-plate and allow the still to cool. Disassemble the cold still and pour the pot liquid, but not the boiling chips, down the drain. Rinse out the column and put it away. You may screw the cap on your receiver and store your alcohol for later use.

A crude estimate of the alcohol content can be made by burning your alcohol distillate. Weigh a Petri dish and record its empty weight, wbefore in your notebook. Tare the balance and add 10.0 g of your distillate, wdist, to the dish and set it alight. When the fire has gone out, weigh the Petri dish again and record this weight, wafter in your notebook. The percentage of alcohol of your distillate is approximately:[2]

[95 - 100(wafter-wbefore)/wdist]%

Double the percent alcohol and you have the proof. If your product is below about 40% alcohol (80 proof), you will be unable to light it at all.

Do not overlook this experience, my brothers and sisters. To merely read and parrot the words is unworthy of your talents. If you are to really live, you must see and feel and know for yourself.

 

It rises from the earth to Heaven and descends again to the Earth and receives power from Above and from Below. Thus thou wilt have the glory of the Whole World. All obscurity shall be clear to thee. This is the strong power of all powers for it overcomes everything fine and penetrates everything solid.

 The Emerald Tablet of Hermes Trismegistos

Scat!

Figure 16-8. The Spirit Lamp

ImportantQuality Assurance
 

You have succeeded in making ethanol fuel when you are able to light your distillate. Your notebook should note the head temperatures at which you began and ended your collection and you should estimate the percent alcohol in your distillate.

Notes

[1]

Reference [32].

[2]

A simple distillation like this one produces a distillate which is, at most, 95% alcohol so we must subtract the percent water from 95 rather than from 100.