And that is why I only reflux for about 10 minutes after equilibrium is achieved when distilling neutral. For rum, 1 hour. Whiskey about 20 minutes. I feel that the stacking doesn't take that long and I also don't just drip out the fores/heads, I go a little faster. I agree that there isn't only a point of diminishing returns on neutral but a point where you are adding flavors.
If we stick to talking about neutral here the conversation will make more sense. Too much confusion will start if we are talking about brown spirits where the entire process and the goal is different.
Have you done the cuts yet popcorn? I meant to say to make your first taste/smell one the center cut for reference and to go first after that to the one you think is the second hearts after heads and work back into the heads. Same process for tails although that should be very simple.
I usually found in the end that my cuts straight from the still were very close.
@grim said:
Regarding automation of cuts, impossible unless you have nearly perfect batch consistency. No sensor is going to tell you what your sense of smell and taste doesn't already know.
@grim: that is really well said! All the fuzz about automation and fully automatic stills - it just is the wrong approach. There are so many always changing parameters that influence the product. Smell and taste may be difficult to judge but this way of doing cuts cannot be omitted.
StillDragon Europe - Your StillDragon® Distributor for Europe & the surrounding area
@punkin - What worked for me early on was using a larger number of smaller jars, and looking for what I called the "neutral break" jar. I've found this to be the case pretty universally, as long as your fractions are small enough. Then, once you've identified that break point, then you can slowly step your way back into heads using the break jar as reference point, and not comparing side-by-side.
This sounds pretty similar to your approach. Comparing side-by-side ends up being much more difficult, especially once you've hit the burn-out point of your senses. Once hit hit burn out, it all goes to a blur. I know you guys like to air out and re-test, and that's good practice, but sometimes it's good to let your senses rest as well. Going in with a fresh nose and tongue the next day makes a big difference.
@punkin I have made my first selection yes, but as @grim was describing I wanted to give my senses a break before I was sure. I was a little to on the fence with my smell-taste test to go ahead and mix everything together. I will point out if I wasn't so against the third run I would just grab my first thinking and move on to the final run and make cut just a little more. I should have my final selection made by this weekend.
Another nice approach is to spend a little money and buy a set of chemicals from a lab supply as references. Every few days smell your way through the references randomly until you can identify each major chemical by smell.
I was randomly buying chemicals as samples, I got most of the ones that are identified with beer off-odors (acetaldehyde for example), and some of the fusel alcohols are very easy to find (isobutyl, n-propyl, isoamyl, etc).
It was really fun to be able to learn the specific chemical odors, and flavors (use common sense) and then reference them back to the distillate or the wash.
Heads a little tougher, but on the tails side, this really helps.
I figured refluxing that long and drawing off at such a slow rate that it might be cleaner tasting. It did stay at 190 though and that I've never accomplished much past the fire shots.
Just a quick note, Furfural - If you are using molasses (esp. Blackstrap), deeply roasted malts, or a direct fired still - this is helpful. Otherwise, sugar or grain washes without Maillard reaction components, you won't get this.
It affects different tastebuds in different ways, but personally I find some cherry cola even more disgusting than normal if mixed with a spirit containing any heads at all. I can't remember who recommended it, but for me it works. Seems to exaggerate the worst aspects of heads.
Acetone ... I'll share because I went down this path.
I think the discussion about acetone is a bit overblown in the hobby community. Acetaldehyde and Ethyl Acetate will be found in significantly higher concentrations. There are plenty of other ketones that would exist with a similar odor that would probably be more prevalent. Fores kind of smell like acetone/paint thinner, so I'm sure this just helped propagate this.
If you look at the literature, you don't actually see much. For example:
Ethanol content ranged from 10.5% to 66.0% with a mean value of 41.2%. Lead was found in measurable quantities in 43 of 48 samples with values ranging from 5 to 599 parts per billion (ppb) with a mean value of 80.7 ppb. A total of 29 of 48 (60%) of samples contained lead concentrations above or equal to the EPA water guideline of 15 ppb. Methanol was found in only one sample at a concentration of 0.11%. No samples contained detectable concentrations of acetone, isopropanol, or ethylene glycol.
Pretty sure that these elicit moonshiners aren't making great heads cuts, despite what the TeeVee says.
So in theory, if you are going slow, once you hit 171 all the bad shit should be gone? My temp sits at 172.5 during the hearts run so that makes sense.
Many of those higher BP compounds will easily come through in the distillate.
For example, all of the organic acids will make it through distillation (as acids), even though their boiling points are far above that of water or ethanol (240F+).
Also, great example of the fact that BP doesn't always mean what we think it does, Isoamyl alcohol, which is Chief Fusel # 1, which doesn't only come over in tails, but in the hearts cut as well. It's got the highest BP of the fusels listed above, which might make you think it should come over in the lowest quantity in comparison ... nope.
Not to mention some of the sneaky things these chemicals can do. Like turn into a highly volatile ester during distillation, and then hydrolyze back to a high boiling point constituents during aging, damn compound ran damn through the toll without paying a dime.
Exactly right! Boiling point is a good indicator at where the chemicals may be present, but the fact is that these are ideal solutions so their partial vapor pressures determine how much actually vaporizes. It will be a smear of the chemicals across the board and what we need to consider is the original concentration and vapor pressure. From that you can determine the vapor concentration of each chemical (Raoult's & Dalton's Laws) in the vapor. But beyond this what you're really after is the quantity required to make an impact on humans both physically and sensorly.
And thanks for that great table. (Look at all that methanol in that Grappa! Heads cuts are over-rated...)
Yeah about that eye thing so I did it on my last run that I was having trouble with the cuts, and well it burned on everyone of the samples just not near as bad as the front ones. Is this your experience also @FloridaCracker
No. If I am at a spot that I think the run is turning, I will use it as a tool along with my nose and taste buds. Something in the heads burn the eye more than hearts.
Enter Grim to explain the science of it in three, two, one......
Comments
And that is why I only reflux for about 10 minutes after equilibrium is achieved when distilling neutral. For rum, 1 hour. Whiskey about 20 minutes. I feel that the stacking doesn't take that long and I also don't just drip out the fores/heads, I go a little faster. I agree that there isn't only a point of diminishing returns on neutral but a point where you are adding flavors.
If we stick to talking about neutral here the conversation will make more sense. Too much confusion will start if we are talking about brown spirits where the entire process and the goal is different.
Have you done the cuts yet popcorn? I meant to say to make your first taste/smell one the center cut for reference and to go first after that to the one you think is the second hearts after heads and work back into the heads. Same process for tails although that should be very simple.
I usually found in the end that my cuts straight from the still were very close.
StillDragon Australia & New Zealand - Your StillDragon® Distributor for Australia & New Zealand
@grim: that is really well said! All the fuzz about automation and fully automatic stills - it just is the wrong approach. There are so many always changing parameters that influence the product. Smell and taste may be difficult to judge but this way of doing cuts cannot be omitted.
StillDragon Europe - Your StillDragon® Distributor for Europe & the surrounding area
@punkin - What worked for me early on was using a larger number of smaller jars, and looking for what I called the "neutral break" jar. I've found this to be the case pretty universally, as long as your fractions are small enough. Then, once you've identified that break point, then you can slowly step your way back into heads using the break jar as reference point, and not comparing side-by-side.
This sounds pretty similar to your approach. Comparing side-by-side ends up being much more difficult, especially once you've hit the burn-out point of your senses. Once hit hit burn out, it all goes to a blur. I know you guys like to air out and re-test, and that's good practice, but sometimes it's good to let your senses rest as well. Going in with a fresh nose and tongue the next day makes a big difference.
@punkin I have made my first selection yes, but as @grim was describing I wanted to give my senses a break before I was sure. I was a little to on the fence with my smell-taste test to go ahead and mix everything together. I will point out if I wasn't so against the third run I would just grab my first thinking and move on to the final run and make cut just a little more. I should have my final selection made by this weekend.
Another nice approach is to spend a little money and buy a set of chemicals from a lab supply as references. Every few days smell your way through the references randomly until you can identify each major chemical by smell.
I was randomly buying chemicals as samples, I got most of the ones that are identified with beer off-odors (acetaldehyde for example), and some of the fusel alcohols are very easy to find (isobutyl, n-propyl, isoamyl, etc).
It was really fun to be able to learn the specific chemical odors, and flavors (use common sense) and then reference them back to the distillate or the wash.
Heads a little tougher, but on the tails side, this really helps.
I stay confused and I am trying to lead everyone else down that path
:))
Has anyone mentioned kiwi guide to cuts, as a visual aid
I have almost memorized that thread. Amazing info in there.
Made the cuts
Kept jars 6-16 giving me 8.5L I fell that compressing and running super slow causes the fractions to bleed through to much
Definitely learned a lot from that run. The end result is still very nice, just not What I was expecting
What didn't meet your expectations?
@grim I really like your idea of buying chemical samples for organoleptic reference training. :-B
Any help with a shopping list greatly appreciated.
I figured refluxing that long and drawing off at such a slow rate that it might be cleaner tasting. It did stay at 190 though and that I've never accomplished much past the fire shots.
Heads
Tails
Just a quick note, Furfural - If you are using molasses (esp. Blackstrap), deeply roasted malts, or a direct fired still - this is helpful. Otherwise, sugar or grain washes without Maillard reaction components, you won't get this.
It affects different tastebuds in different ways, but personally I find some cherry cola even more disgusting than normal if mixed with a spirit containing any heads at all. I can't remember who recommended it, but for me it works. Seems to exaggerate the worst aspects of heads.
For what it's worth here are the boiling points of the above:
And what about acetone (132.8°F). I always thought that was in the heads as well??
Acetone ... I'll share because I went down this path.
I think the discussion about acetone is a bit overblown in the hobby community. Acetaldehyde and Ethyl Acetate will be found in significantly higher concentrations. There are plenty of other ketones that would exist with a similar odor that would probably be more prevalent. Fores kind of smell like acetone/paint thinner, so I'm sure this just helped propagate this.
If you look at the literature, you don't actually see much. For example:
Analysis of moonshine for contaminants @ NCBI
Pretty sure that these elicit moonshiners aren't making great heads cuts, despite what the TeeVee says.
This is the only really decent reference to acetone that I could find:
Moonshine Markets: Issues in Unrecorded Alcohol Beverage Production and Consumption @ Google Books
So in theory, if you are going slow, once you hit 171 all the bad shit should be gone? My temp sits at 172.5 during the hearts run so that makes sense.
Many of those higher BP compounds will easily come through in the distillate.
For example, all of the organic acids will make it through distillation (as acids), even though their boiling points are far above that of water or ethanol (240F+).
Also, great example of the fact that BP doesn't always mean what we think it does, Isoamyl alcohol, which is Chief Fusel # 1, which doesn't only come over in tails, but in the hearts cut as well. It's got the highest BP of the fusels listed above, which might make you think it should come over in the lowest quantity in comparison ... nope.
Not to mention some of the sneaky things these chemicals can do. Like turn into a highly volatile ester during distillation, and then hydrolyze back to a high boiling point constituents during aging, damn compound ran damn through the toll without paying a dime.
Kinda like transporting wort to the distillery rather than beer aye!
StillDragon North America - Your StillDragon® Distributor for North America
@grim +1!
Exactly right! Boiling point is a good indicator at where the chemicals may be present, but the fact is that these are ideal solutions so their partial vapor pressures determine how much actually vaporizes. It will be a smear of the chemicals across the board and what we need to consider is the original concentration and vapor pressure. From that you can determine the vapor concentration of each chemical (Raoult's & Dalton's Laws) in the vapor. But beyond this what you're really after is the quantity required to make an impact on humans both physically and sensorly.
And thanks for that great table. (Look at all that methanol in that Grappa! Heads cuts are over-rated...)
You said it better than I could
Damn! So I have to keep sticking my eye in it after all.
Yeah about that eye thing so I did it on my last run that I was having trouble with the cuts, and well it burned on everyone of the samples just not near as bad as the front ones. Is this your experience also @FloridaCracker
No. If I am at a spot that I think the run is turning, I will use it as a tool along with my nose and taste buds. Something in the heads burn the eye more than hearts.
Enter Grim to explain the science of it in three, two, one......
I'm just imaging you guys with your doodle hanging in a glass of heads and screaming about the burn in the eye.
At 2:10
https://www.youtube.com/watch?v=zr6HsSmDcbk
StillDragon Australia & New Zealand - Your StillDragon® Distributor for Australia & New Zealand
Some dude is laughing in his grave about making up the eye thing one day as a joke.