Still Head Temperature For Making Moonshine – When To Start And Finish Collecting – Knowing when to start collecting moonshine from your still and when to finish is very important. You will often start to see some product dripping from your still when the Head / Column temperature reaches 56 Celsius.
But generally the temperature range that you want to collect Moonshine within is between 78-82 °C and we generally stop collecting the distillate once we start getting fusels coming out. This is generally happens at a head temperature of 94 °C or higher. To Learn more about the process of Making Moonshine Head over to our page.
: Still Temperature Guide For Making Moonshine
- 1 What temperature should distillate be collected?
- 2 What temperature are moonshine tails?
- 3 How hot is too hot for distillate?
- 4 Can moonshine be distilled twice?
- 5 Do you put hot or cold water in a distiller?
- 6 At what temperature does methanol distill?
What temperature should I distill moonshine?
Temperature Safety When Distilling – Distilling alcohol uses high temperatures – generally around 200 degrees Fahrenheit. High temperatures mean opportunities for accidents, so make sure that everyone who is in your distilling environment is aware of how hot your equipment will get. Controlling and monitoring the temperature will help you keep your distillery safe.
What temperature should distillate be collected?
First Distillation of Fermentation Mixture – After the fermentation is complete, you will distill the alcohol from the liquid mixture, including the solid, particulate material that is not soluble. Gently pour all of the liquid into a 500-mL round-bottomed flask (checked out from the stockroom).
The liquid will be somewhat cloudy, but this will not interfere with the first distillation (do not ever let a distillation flask go dry, but this should be of little concern here since we will only collect a fraction of the liquid via distillation). Add a few (6-8) boiling stones to the flask. Attach a fractional distillation column (filled with glass beads, as described in Part B ) to the top of the distillation flask, and attach the still head and condenser unit.
You do not need to monitor the temperature as the first distillate is mostly water, so the temperature will be about 100 o C. Collect about 50 mL of distillate into a pre-weighed graduated cylinder (a 50- or 100-mL graduated cylinder can be used). After the first distillate has been collected, observe and record the collected volume, and weigh the graduated cylinder to determine the mass of collected distillate (total mass of cylinder containing the distillate minus the mass of the empty graduated cylinder).
- You should now calculate the density of the distillate, based on the mass of the distillate you just determined divided by the volume collected.
- From the Table of Densities of aqueous ethanol solutions, given in Footnote 2, calculate the mass of alcohol collected in this first distillate.
- To make your determination of the amount of ethanol isolated, you can estimate your percent alcohol using the table at the end of this experiment.
This table shows you several ways to determin the amount of ethanol in your sample based on density. The easiest column to use is the first column which shows the mass percent of alcohol (% by mass) as follows: Using the density of your distillate from the above calculations, determine the percent alcohol ( you may have to extrapolate (e.g., Calculate the percent yield of ethanol produced in the fermentation, based on the theoretical amount of ethanol that would be produced from the starting amount of glucose (each glucose molecule produces two ethanol molecules).
This “crude” distillate will be used in a second fractional distillation. An additional table is available, using an interpolative procedure to determin percentages which do not fall within the larger percent range shown in the table below (percentages are in 5% increments). The new table (which is an Adobe pdf document) shows you how to get to the percent values, based on density, in unit values, e.g., 45%, or 46%, or 47%, etc.
The highlighted values in this pdf document shown how to determine percent concentration values between 45% and 50% ethanol. You can download and print this document at this URL of a pdf document, Discard the residue left in the distillation pot, which contains mostly water.
- One can obtain 95% ethanol (but not 100% ethanol; do you know why? What is an azeotrope?) from the dilute alcohol mixture obtained during the first distillation.
- For the second distillation, monitor the boiling point carefully, as you should collect the material that distills at a temperature of 78-82 o C; if too little distillate is obtained in this range, continue the distillation and collect the fraction boiling at 82-88 o C.
Prior to doing your second distillation, empty the glass beads from the fractioning column into a beaker you will wash them yourself with soap and water, and then reuse them. Also, you need to wash with soap and water each of the following pieces of glassware:
- Fractionating column
- Still head
- Condenser column
You can now re-assemble your distillation setup for a fractional distillation, and then follow the procedure for collecting and analyzing your second-distillate liquid. At the end of the experiment, put the used glass beads into a beaker on the Instructor’s bench to be washed by the Stockroom Personnel.
- Add the alcohol-water mixture from the first distillation (after weighing and determining its density) to a 100-mL round bottom flask.
- Add a few boiling stones to your round-bottom flask (distillation pot) to maintain a slow, steady boiling.
- Start monitoring the temperature as soon as you turn on the heat, or at least prior to the solution boils. Monitor the temperature at regular intervals, usually every minute, until you stop collecting your samples.
- Start to collect 4-mL samples (using you conical vial in the organic kits or a test tube) until the temperature rises significantly above the normal 78-82 o C temperature, as described above. It is still permissible to collect above the 82 o C degree range, but your samples contain more and more water. However, if you have not collected at least 4-5 samples, each of about 4-5 mL volumes, continue to collect samples (regardless of temperature) until at least 20 mL of solution is collected. Based on theoretical yeields, and actual lab experience, you could have produced 30-36 mL of ethanol during your fermentation, so collectin at least 20 mL is not out of reason.
- Do not determine a refractive, but you must determine a density for each sample. To do this, collect about 4-5 mL in a conical vial (as mentioned above), and then immediate transfer the contents of the vial into a pre-weighed 10-mL graduated cylinder. After transfer of collected material into the 10-mL graduated cylinder, reattach the vial to the vacuum adapter, and collect another 4-5 mL sample.
- Determine the mass and volume of the sample in the 10-mL cylinder to calculate a density of the sample. After determining the mass and volume, transfer its contents into a pre-weighed 50-mL graduate cylinder to collect all samples for an overall density and yield of ethanol for the entire experiment.
- After you have analyzed individually the 4-mL samples, combine your 4-5-mL collected distillate samples into the 50-mL graduated cylinder, the total volume, the mass of the sample in the 50-mL cylinder, you can determine the density.
- From the density just determined (step #7), determine the total mass of ethanol collected during the second fractional distillation. No need to determine a refractive index as density (and total mass of solution) will be our criterian for yield.
- Determine percent yield based on the overall yield from step #8, by dividing the actual yield by the theoretical yield times 100 to get a percent yield.
Based on the amount of collected alcohol, its density, what is the percent yield? What is the theoretical yield?. Your instructor will help you determine the percentage of alcohol based on your refractive index and density determinations. Do not throw any glass beads away.
What temperature are moonshine tails?
Finally, at around 205°F, the tails condense out. Like the heads, these contain some unpalatable flavors, so they’re usually removed from the rest of the distillate. Because water boils at 212°F, the tails are mostly water and will dilute the rest of the spirit if not cut properly.
How hot is too hot for distillate?
Distillate can be warm as long as it’s not 100F or more.
What is the minimum temperature difference for distillation?
Simple distillation (the procedure outlined below) can be used effectively to separate liquids that have at least 80℃ difference in their boiling points. As the liquid being distilled is heated, the vapors that form will be richest in the component of the mixture that boils at the lowest temperature.
Is temperature important in distillation?
In conclusion, good temperature measurement and control practices are critical to efficient, safe and profitable operation of distillation and fractionation processes.
Can moonshine be distilled twice?
The Distillation – Distilling Alcohol – For distillation use the entire mash, both liquid and solid parts. Don´t filter the mash before distilling. You would lose taste and smell by filtration. Therefore the stills contain solid parts. Hence it is necessary to use a burn protector, Large stills are jacketed kettles in common, mostly equipped with a stirrer, but this system is not appropriate for small copper stills of hobby distillers. If the mash contains less than about 10 %ABV alcohol, you have to distill twice (double distillation). If the alcohol content is higher than that, a simple distillation is completely sufficient. This kind of distillation produces the most intense taste and smell, more than double distilled alcohol. Don’t forget to separate the heads (foreshot). Also if your mash is free of heads, you should separate about 30 drops per 1,5 liters (1.5 US quarts) of mash. Collect the hearts until 91 °C (196 °F) steam temperature, after that you can collect the tails or stop the distillation.
At what proof do you stop distilling?
How to Take Cuts During Distillation Learning how to take cuts during distillation may seem like a daunting process to begin with but by following some basic steps and getting some practice, you’ll be a pro in no time! Taking cuts refers to the process where spirit is collected in small portions of similar sizes during distillation as opposed to allowing the distillate to collect in just one large vessel.
This process gives you more control over the flavours and aromas that make it into your final product, allowing you to create something truly unique and to your taste. During fermentation, many compounds are produced along with alcohol such as acetaldehyde, esters, and ethyl acetate. By taking cuts, we can minimise how many of these by-products make it into our final spirit.
Some of these by-products appear earlier on in the distillation, and others come out later or towards the end of the distillation – this depends entirely on the compound itself. Not all these by-products are bad. Some do not taste wonderful on their own, however, it can be beneficial to introduce them in small amounts to contribute different attributes to your final spirit.
The foreshots are the first part of the distillate (usually 50-200 mL depending on what is being distilled) which are discarded as these can contain harmful compounds and off-flavours. The heads are the distillate collected immediately after the first 50-200 mL of discarded foreshots. They can contain some undesirable, but not harmful, compounds and off-flavours. Some of these are blended into your final spirit, however, most will be discarded or retained in a separate container for redistilling in future batches. The hearts are the middle part of a run and are the cleanest and most flavoursome part of the distillate. A minimal amount of undesirable compounds come through into the spirit. They make up the bulk of your final spirit. The tails are the final part of the distillation and contain some vegetal off-flavours. These are also typically discarded, however, like the heads they can also be kept in a separate container for redistilling.
The Stripping Run The stripping run is done first and ‘strips’ the wash down to a cleaner, more concentrated low wine. This distillation is usually done hot and fast, meaning temperature control isn’t as important as the aim is to strip the wash quickly. Just be sure to take care not to run it too hot to avoid the loss of vapour from the condenser.
The purpose of a stripping run is to capture as much distillate from the wash as possible, therefore, there is no need to remove the foreshots (50-200mL) as these can be removed during the spirit run. The Spirit Run Once you’ve completed the stripping run, it is then diluted with water to 40% ABV or lower and then distilled again – this is where cuts are taken. During this distillation run, the flow of the still should be kept slower than on the stripping run, and ideally, the voltage going to the boiler should be controlled to ensure a nice gentle boil – the is a great example of a boiler that can double as a brewing system to make Whiskey and Bourbon washes, and then control the voltage during distillation. How to Take Cuts During Distillation
There are a few different methods to work out how to split and collect the different cuts from a spirit run, some people base it on temperature or ABV, while others evenly split the whole run and then taste and smell later. Either way can work but to simplify things, we’re going to talk through splitting the entire run.
- To do this, you will need an adequate number of glass jars, preferably 300-500 mL in size, that will be able to collect the entire run – this amount will depend on how many stripping runs have been done, if it is only one, then approx.24 x 400 mL jars should suffice.
- For best results, number these so you know where exactly the cut was made.
The next step is to fire up your pot still and get ready to start the process. You will need to discard the foreshots as usual. Depending on how many stripping runs you have done this could be anything from 50 to 200 mL. Once the foreshots are discarded, you can start collecting the remaining distillate into the jars.
Ensure you collect the same volume into each jar (250 mL – 300 mL is usually a good figure – you can test and adjust this to suit your still later) and then set the jar aside. Depending on what you wish to do, and what you’re making, you can stop collecting the distillate once the ABV drops to 10% or below, although some stop it even higher.
You may start to notice some more visible by-products forming in the last number of jars – this could be an oily looking substance or off-colours coming through. We then suggest you let the jars air out for 24 hours for the more volatile aroma compounds to dissipate.
At what temp does distillate degrade?
Posted on 17 August 2019 By Goldleaf Scientific Posted in Purification 0
Because cannabinoids themselves have a high boiling point and would foul or degrade when exposed to high temperatures vacuum is applied to lower the boiling points. If you are not able to achieve a deep enough level of vacuum whether through leaks, poor vacuum pump performance, or other ways the temperature needed for distillation to take place is increased.
- As temperature is increased the degradation of cannabinoids becomes increasingly greater.
- Generally, temperatures above 245°C lead to increasing degradation and this should serve as the upper limit for recommended temperatures to distill.
- Temperatures higher than 245°C leads to an increase in cannabinoid degradation products like CBN, and especially delta-8-THC.
At temperatures above 260°C more than 50% of cannabinoids can be converted to these degraded cannabinoids and other unknown compounds. If, however a heavy vacuum leak is in your system and is exposed to these temperatures a much heavier degradation will take place.
- A complete loss of cannabinoids is possible as they polymerize at high temperatures and exposed to oxygen.
- They will turn into a solid that is very hard to remove from the flask.
- In general oxygen should be limited as it will degrade the oils.
- Back-filling flasks, containers, and the complete distillation system with inert gas wherever possible is recommended.
Exposure to acids, light, metals, heat, and oxygen or oxidizers will cause degradation. Use of activated absorbents can also cause degradation if combined with the oil and exposed to high temperatures. It should go without mentioning that adding absorbents to the boiling flask and distilling with them will lead to heavy degradation.
Depending on the level of activation, amount of absorbent used, and temperatures the level of degradation can vary. The absorbents work best at lower temperatures and any reduction in color associated is likely caused by the breakdown of compounds. Those that have added adsorbents to the boiling flask and distilled have noted a heavy blue fraction and this is likely an indication of the breakdown of cannabinoids.
Also noted is a conversion of cannabinoids into CBC. Oil begins to rapidly break down when exposed to air after this initial heavy degradation. A color change from colorless or yellow to pink or red after exposure to air indicates that the sample is oxidizing and the rate of which indicates the level of initial degradation, or put another way, the more degraded the sample the quicker it will oxidize after exposed to air.
- Samples that are heavily degraded can change from colorless to pink in less than 24 hrs.
- Cannabinoids have antioxidant properties and are initially somewhat resistant to chemical breakdown, but eventually they will degrade and once that process has begun it will accelerate.
- In order to attain an acceptable shelf life, potency, and consistency one must always seek to find method to limit or reduce breakdown and oxidation.
It also must be noted that in order to make clean distillate without any issues you must first winterize (de-wax) your sample.
Do you put hot or cold water in a distiller?
Extreme coldness. It’s what makes Duluth, Duluth. Our partisans (see: Emily) call it “pristine,” and “wild.” They say it makes them proud to live in Duluth. It makes them feel like they earned it. As a relatively new Duluthian, whose brain hasn’t been through too many freeze-thaw cycles, I just call it “ridiculous.” It makes me feel braveon the days when it doesn’t make me feel scared. As a distiller, the cold is an inescapable physical reality. When it’s -30F outside, which is a regular operating condition in Duluth, mechanical systems work differently. The diesel in our distillery truck turns to jelly. The cold air in our chimney is too heavy for the hot exhaust gases from our boilers to fight through, so instead of rising, smoke just pours out into our mechanical room.
- That’s if the boiler isn’t too frozen to fire at all.
- In the winter of 2013 our boiler partially froze, and Canal Park Brewery’s boiler partially froze, and Bent Paddle Brewery’s boiler froze solid – all in the same week.
- It was one of those scary weeks.
- The primary distiller’s downside to cold is that it slows barrel aging.
This is part of why Kentucky Bourbon ages in 5 years but Scotch whisky takes 10. Whisky in Scotland basically takes the winter off from aging. But mostly, for a distiller, cold is a good thing. Because distilling is about boiling and condensing, and the condensing takes cold. condensers on the still Here in Duluth, we have cold water year round. Our tap water comes from Lake Superior, which is ridiculously cold. In the winter it comes out of the tap around 40 degrees. In the summer it runs around 50 degrees. So when we began, we began by using this cold water to do our condensing.
- This was an energy efficient choice, but not a water efficient choice.
- In the last year we’ve been using as much as 200,000 gallons of water a month, and while this is not at all an unusual amount for a distillery, it was not a resource use we felt good about.
- So when we came up with our strategic plan for 2015, we set a goal of reducing our water use by 50%.
Given Duluth’s extreme cold, you’d think cooling process water would give you an embarrassment of options. Over the last year, I’ve investigated many many options. I considered an open cooling loop to the lake. I considered a closed loop with a heat transfer coil in the lake.
- I considered a closed geothermal loop digging down from an old storm sewer under the distillery.
- I talked to engineers, to engineering professors, to engineering students, to geothermal contractors, to industry cooling contractors, and to process water experts.
- I called every imaginable resource, including the city, the utility company, non-profits that specialize in energy use reduction and making manufacturing more environmentally friendly.
But, mostly they suggested solving the problem with electricity by mounting a big old electric chiller on the roof and calling it a day. This would mean running a big compressor all year long to create cold – in an atmosphere already overflowing with extreme coldness! This, interestingly, is the way almost all breweries do their cooling, even in cold places like Duluth.
But, this did not satisfy me. I did not want to reduce our water use by dramatically increasing our electricity use, particularly given that most of our regional electricity comes from coal. So, I kept talking with people until, I found a couple folks willing to help. One is a process cooling specialist from Alabama, and the second is a civil engineer in Duluth.
This is what we did (in case you’re interested): Our cold process water runs through the condensers on the stills, and the fermenting equipment (more on our fermenting equipment – which we affectionately call “the brewery” – soon!). It comes out hot. This hot water runs over to our barrel room, and through a few refurbished fan coil units.
These are basically just radiators with fans that we found in a basement, and they push some of the heat out of the water and into the room. This means the barrels get heated up during the day when the stills are running, and then cool off at night. In the winter it’s enough heat to keep them around room temperature instead of freezing.
In the summer it’s enough to make the barrel room miserably hot. This diurnal variation is exactly what we want to facilitate whiskey aging. the radiator in the barrel room Then that still-quite-warm water runs back over to the distillery and into a 2,000 gallon reservoir. From the reservoir, the water is pumped through a heat exchanger where it’s cooled off, and then back out to the distillery and brewery process. All in a nice closed loop. the heat exchanger and pumps Now the heat exchanger works by transferring the heat from the water to a second medium, which is glycol. The glycol (basically food-grade antifreeze, and a key ingredient in Fireball™, hehe) is pumped through the heat exchanger, and it takes on the heat from the water, before it runs up to a hybrid adiabatic cooler on the roof.
- What the heck is a hybrid adiabatic cooler, you ask? It is essentially just a giant radiator with a fan.
- Most of the year, given our extreme cold, that’s all it takes to shed the heat.
- In the summer, when the ambient temperature is higher than we want our process water to be, the cooler sprays water into the air as it passes through the radiator, allowing it to shed a couple extra degrees.
That’s the “adiabatic” part. We benefit here from the fact that it stays pretty cool on the lake even in the middle of the summer, and it’s almost always windy up on our roof. The glycol leaves the cooler, well, cooler, and comes back down to the heat exchanger to take on some more heat from the water. roof top cooler unit The water reservoir allows us to store cold, and to buffer changes in the temperature of the process water, which can really mess with the distilling process. By the end of the day, the reservoir will be pretty warm, but overnight it cools back down so in the morning we have nice cold water to start with. This allows us to run a smaller system than we otherwise would. water reservoir We’re still in the first month of operating this cooling system, so the numbers are still shaking out. I think we’ll have reduced our water use by about 90%. And we’re still getting the controls hammered out so it can efficiently regulate itself. Lake Superior
At what temperature does methanol distill?
Why is Methanol A Concern for Distillers? – If wine contains methanol but doesn’t pose a risk of methanol poisoning then why is it potentially dangerous to drink once distilled? The difference is that the methanol concentration in, say, 5 gallons of wine, is evenly distributed among the 5 gallons.
- For someone to ingest a potentially dangerous amount they would need to ingest more than 5 gallons.or 28 bottles! During the distillation process methanol is concentrated at the start of the production run because it has a lower boiling point than ethanol and water.
- The boiling point of methanol is approximately 148 degrees farenheit, which is quite a bit lower than ethanol (the good stuff).
This means that methanol (148F boiling temp) will start to boil before the ethanol (174F boiling temp). This is why commercial distillers always throw out the first bit of shine they produce from each production run (more on this below). Here are a few examples of the dangers of methanol :
If 5 gallons of wine containing the abovementioned concentration of methanol (329mg/L) were distilled, there could be as much as 8 mL of methyl alcohol in the first jar – a potentially dangerous amount. Scale this up to a 100 gallon batch, distilled all at the same time in a large still, and a commercial distiller could potentially have a very big problem if the methanol was not discarded. Distilling 100 gallons of wine containing 329 mg/L of methanol could result in the concentration of 40ml of methanol, which could be fatal if someone drank it all at once.