To know how something works, it is essential for us to know about the ultimate purpose of that thing, and in this case, we need to know about
the reflux distillation technique. In simple terms, this technique involves the condensation of vapors and the return of this condensate to the system from where it originated, and this magic is definitely worth your time on a homemade still!
With an idea of what this is about, let’s move forward on how to operate the still. So, first things first! Before you start your adventure, safety is what you need to keep in mind. The process may involve you in working with heat, steam, gas, electricity, and explosive vapors therefore you need to be very careful while executing the technique!
Prevention is better than cure, and in this case, it is better that you test your apparatus by distilling some water, probably a gallon or two, to make sure that the apparatus is free of any loopholes which, otherwise, may cause potential harm to you and the apparatus. This test would ensure some of the essential things, such as, there is enough heat to boil the liquid, and the joints don’t leak, that there is enough cooling to control the distillation. Moreover, it would also clean up any flux from the joints soldered during construction. For further information, visit: http://www.che.ufl.edu/ren/course/4404L/CD/CD.pdf.
Start off by pouring a gallon of tap water into the boiler and by mounting the boiler on top of the heat source. Once you are done with this, attach the column to the boiler. Then, attach the cooling hoses on the column to the water supply and drain. At this time, however, do NOT let the cooling water circulate the apparatus. Your next step is to turn on the heat to its highest setting and insert the thermometer in the top of the column, where the bulb should be resting on the level of the upper column tee connection – the point where vapor flows into the condenser.
In some time, approximately 10 to 15 minutes, the water should be boiling to the point where vapor and liquid could be observed exiting the condenser and the thermometer should indicate that the temperature has reached up to 100° C. (This temperature may vary with different liquids as it corresponds to the boiling point of the liquid poured into the boiler)
It is now time to determine the maximum distillation rate of still. In order to do so, open the cooling flow to the maximum. On the other hand, increase the boiling rate to the point where the condenser fails to condense the entire vapor.
At this point, slowly back down the heat until the vapor can no longer exit the condenser, but do not drop the heat so that the temperature drops below the boiling point, which in this case is 100° C. You will now be at the maximum distillation rate settings for the still. Upon reaching this point, measure the time it takes to collect 250 ml of the distillate precisely.
But why do we need to know the maximum distillation rate? It is so because it forms the basis while estimating the reflux flow. Note that for different liquids, you will need to repeat the exercise each time.
After a successful execution of the process, it is equally important to successfully conclude the process. The fact that the process is very simple complements the fact that the still is a homemade still. The following is the shutdown sequence:
1. Remove the thermometer cap from the top of the column. (You may use gloves as it might be hot)
2. Turn off the heat.
3. Finally, shut off the cooling water circulation.
The sequence is important because the tubing used to collect the distillate might get obstructed, sealing off the apparatus from air. If this
happens while it is cooling down, a vacuum would be formed within resulting in the crushing of the still by external air pressure.
Once the still reaches room temperature, you should disconnect the cooling hoses, back-flush the column with water, remove the cover and clean the boiler. With this step, you are finally through!
For more information, visit: www.stilltutorial.com.
Note: Remember, the distillation of ethyl-alcohols is illegal without a permit per federal moonshine laws and is inherently dangerous because of ethanol’s flammability (never operate a homemade still indoors). For more moonshine laws and other moonshine still permit information, visit: http://www.ttb.gov/spirits/faq.shtml. Sorry, ya even need a license for personal use due to TTB federal distillation moonshine laws.
For more info on your own homemade copper still plans for home, see http://stilltutorial.com