Capsaicin Distillation From Nuclear Peppers
The goal is to use the excess powder created from this year's nuclears (Bhuts, Butch T's, and Douglahs) to produce concentrated capsaicin crystals.
The Goods
These are my starting ingredients and tools. We have:
1 bottle of nuclear pepper powder
1.75 liters of 190 proof alcohol
1 (case) Medium sized canning jars (will only use one though, can't buy just one of those things though)
1 canning funnel
1 package coffee filters
1 oversized novelty martini glass
1 photo bombing cat (optional)
The Theory
The chemical that makes peppers hot, capsaicin, is a hydrophobic molecule (meaning it repels water). This is why drinking water only spreads a burn around in your mouth, the water only causes the "oil" to spread around more evenly. To actually dissolve capsaicin you need a non-aqueous solvent, in this case ethanol. By reducing the moisture content to nearly zero (dehydrating your peppers) and increasing the surface area as much as possible (making them into a powder), one can then soak hot peppers in solvent (alcohol) to dissolve the capsaicin into the liquid and then evaporate it off to leave behind the (relatively) pure capsaicin in crystal form (basically like making rock candy out of sugar dissolved in water).
The Practice
First off, I take the pre-powdered nuclear peppers and dump them into my canning jar. One coughing/sneezing fit later, we have most of the powder in the jar, and the remainder on the inside of my nose.
Next up, our solvent. Ideally you'd want as pure of a solvent as possible, like hexane, but that stuff is expensive. Instead, I hit a local liquor store and obtained some "food grade ethanol", aka 190 proof grain alcohol. This one happens to be Golden Grain brand. Many warnings here, this stuff is crazy dangerous. Do not drink this stuff straight, and don't get it near fire. It burns with an invisible flame and can easily explode if the main container is near an open fire or extreme heat source. An invisible explosion. Seriously, you'd have to be brain damaged to drink this stuff, and if you weren't when you started you probably will be by the time you finish it. Just say no to this stuff, just use it as a solvent and pour it in the jar enough to fill it and give it a good shake to mix it up.
Now ideally you are supposed to have at least a 7:1 ratio by volume of solvent to powder for this, but my evaporation vessel is a little small, so I will be running multiple rounds of solvent through the pepper mash to make up for the higher concentration.
Once the jar is filled and thoroughly agitated to mix it (shake the living bejeezus out of it), set it in a cool dark place (like the cupboard) for a couple of days to let it soak.
Right now, this is as far as I've gotten.
Next Steps
Let the jar sit for a few days, shaking occasionally to keep it well mixed. After those few days have passed, prepare your "evaporation vessel".
Yes, I mean the giant martini glass. Why did I pick a giant martini glass for this? Two reasons. One, it has a very wide mouth which will allow for a very large surface area during evaporation. The more surface area on the liquid, the faster it will evaporate. Two, it tapers down to a point. Like rock candy, the thicker the mix gets while evaporating down, the more it will start to form crystals. As the "water" level drops, it will help concentrate any crystals that form along the wall to the middle area. Means you'll only have to scrape out a little bit of the container instead of the entire thing.
Next, get the funnel and the filters ready.
These filters fit very nicely into the canning funnel I found. I will pour the mixture from the jar through the filter to remove any particulates (aka the powder mash) so that we get only pure alcohol and capsaicin in the evaporation vessel (now you see why I keep calling it an evaporation vessel, "pour your booze in the giant martini glass" just doesn't sound as sciency).
Long slow evaporation makes for bigger crystals (which are in turn easier to collect), and I plan on using the long evaporation period to my advantage. Once the jar mixture is filtered into the glass, I'll scrape the mash off the filter and back into the jar. Pour in a fresh batch of solvent, and then let it soak while the first glass full evaporates down.
Ideally by the time the glass evaporates, the jar will be ready to be poured out again. I'll repeat this until either I run out of solvent.
Judging by how much I have left in here, I'll probably be able to do that a half dozen times, which is most likely overkill. Change of plans, I'll do it 3 times and then give the mash a taste test. If my tongue survives the experience, I'll know its pretty much done.
I could speed things up a bit by heating the evaporation vessel to speed up the evaporation, but I have a few reasons why I don't think thats a great idea.
One, as I already said, slow evaporation means gradually increasing concentrations of capsaicin until it reaches saturation and starts to fall out and form the desired crystals. The slower the evaporation, the greater the odds of having a few big crystals form as opposed to a sheet of tiny crystals.
Two, its a plastic martini glass. I'd have to find some way to get the heat up under the glass while avoiding the stem base, and make it so that there was zero risk of melting the plastic.
Three, the solvent is insanely flammable and explosive. Dissolved in this explosive liquid is pure capsaicin. I don't know about you, but the thought of this stuff burning or exploding and spraying that stuff everywhere may very well give me nightmares tonight.
Four, the evaporation process is going to be freaking outside. If I let a half gallon of 190 proof vaporize in the house, I don't know if I could drive to work in the mornings. The glass I can just set out under the carport, maybe put a little cage around it to keep a bird from flying into it, and just not worry about it until its almost dry. Lot less work to set that up than trying to fix up a heating pad or something like that.
---
Pictures of phase two in a couple of days!
Comments (64)
DMForcier
11 years agolast modified: 9 years ago'Course, if you wanted to speed up the extraction process, you could light it. Shouldn't affect the temperature of the extractate (is that a word?) much so long as there's a fair volume. And you can snuff it with a lid ...
Don't do it in the house.
fusion_power
11 years agolast modified: 9 years agoThe easiest way to "speed up" the evaporation would be with a light bulb. Put a 60 watt bulb under a cardboard box about 2 cu ft capacity. Sit the container of extract in the box. Leave a hole about an inch diameter for vapor escape. The bulb should increase the temperature about 30 degrees above ambient inside the box. A thermometer remote inside the box would allow you to verify the temperature.
DarJones
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11 years agolast modified: 9 years agoVery cool! Thanks for sharing the process with us, looking forward to the updates.
My first thought was "cool!", next was, "what the he11 would you do with that concentration of pure hot?!?!" haha! I'm thinking could just wave the jar over your pot/skillet (without even opening it) and it would impart a fair amount of heat do whatever you're cooking!
Edymnion
Original Author11 years agolast modified: 9 years agoOkay, after one day of unaided evaporation, I already have some results happening.
The white stuff appears to be nothing but a skim, not entirely sure what it is though. The pink stuff, however, is definitely three dimensional (looking from the side of the glass you can see it extending down into the liquid). I've made sure to keep a mesh cover on this to keep anything from falling in, so whatever this is it has to be condensate from the liquid itself evaporating off.
Emboldended by this, I have dug out my scented candle warmer (basically a small hotplate that only gets warm enough to just barely melt wax, you can stick your finger in the melted wax without it hurting) and put the glass on that. Should speed things up quite a bit.
DMForcier
11 years agolast modified: 9 years agoFor those grad students and forensic teams investigating the madness, it actually began in another thread.
Here is a link that might be useful: What the %^$&) is wrong with you?!?
Edymnion
Original Author11 years agolast modified: 9 years agoSo its been sitting on the candle warmer for a couple hours now, and the floaters have disappeared, which is what I expected. Hotter solutions have higher saturation points than colder ones. It does prove that what was floating in there earlier was indeed condensate from the liquid itself, not foreign contamination.
DMForcier
11 years agolast modified: 9 years agoRemember, too, that you're going to get more than capsaicinoids out of the powder: just about anything that is ethanol soluble, plus some that is water soluble in the 5% water.
mbellot
11 years agolast modified: 9 years agoEd - You've inspired (infected?) me with your project.
I was out of town on business the last couple days and just happened to wander into a liquor store... Long day. :)
Walked out with a shiny new bottle of EverClear.
I'm going to grind up all of last season's Bhuts and give this a whirl.
esox07 (4b) Wisconsin
11 years agolast modified: 9 years agoEdymnion
Original Author11 years agolast modified: 9 years agoIt is actually been really interesting so far.
First batch had evaporated down by about half (with no signs of crystallizing again at the higher temperatures) and the soak on the second batch appeared complete, so I just got done pouring the second round into the evaporation vessel and putting it back on the candle warmer. Poured the third batch into the mash jar and put it down to soak some more.
Using the candle warmer was definitely a good idea though. It keeps a nice steady temperature that is low enough that there is zero chance of ignition, but still high enough to really speed things up.
I'm not expecting to see anything spectacular in the morning, but I'll know that its there. Slowly gaining it's strength, laying low until I let my guard down before sneaking up on me in my bed and jumping in my mouth and making me wish for the sweet release of a death that will never come...
Okay, its not going to stalk me in the night, maybe its time I go to bed. =P
DMForcier
11 years agolast modified: 9 years agoWe are nearing the day when the dead and non-living walk. How are your dreams recently?
Edymnion
Original Author11 years agolast modified: 9 years agoWell, in all fairness my dreams at this point are probably being affected by having a pint of 190 proof vaporizing in the house at all times.
lazy_gardens
11 years agolast modified: 9 years agoConsidering that capsaicin is a known cause of chemical burns in concentrations under what you are trying to produce, and skin exposure can cause severe and long-lasting nerve damage (makes you sensitive to heat), eye contamination can cause cornea lesions, inhalation can give you chemical burns to the lungs ... what are your plans for using this stuff?
http://npic.orst.edu/factsheets/Capsaicintech.pdf
https://www.caymanchem.com/msdss/10010743m.pdf
Do you have a disposal method planned, or are you going to call 9-1-1 and have a HAZMAT incident?
Edymnion
Original Author11 years agolast modified: 9 years agoI intend to bottle it, seal the bottle with wax, and then probably set it on my shelf as a novelty.
fusion_power
11 years agolast modified: 9 years agoI suggest that you put yourself in the bottle, seal it carefully, then leave the capsaicin crystals for someone else to find while you relax in your bottle.
DarJones
mbellot
11 years agolast modified: 9 years agoEd - I've joined the crazy train, but I'm all in for one load.
I put ~ 4 ounces (by volume) of Ghost powder into a quart mason jar and covered it with 750ml of EverClear.
Mine isn't as deep red as yours, but it's only been about an hour.
I am curious if it would be possible to recover the evaporating liquid for reuse... It's not cheap, but I'm not sure if that particular type of recycling would run afoul of the authorities. LOL
Edymnion
Original Author11 years agolast modified: 9 years agoYou should be able to get a length of small copper tubing at the hardware store, bend it over half way, coil one side, and connect the straight end to the narrow part of a funnel that you tape down over the main evaporating vessel. Have the other end go into a second jar to reclaim the alcohol.
You really would be distilling then.
mbellot
11 years agolast modified: 9 years agoEd - I get the basic science, I'm just sketchy on the legal aspects. :)
Mine is definitely lighter colored, but I would guess that has to due with the ratio of peppers to solvent. I'm running ~ 1:6 by volume. I'm going to give it a couple days to soak and see how the debris at the bottom looks.
On a related note, I started doing some reading and it's not clear to me if we'll end up with cap crystals... From what I've found we will be creating a oleoresin, or very concentrated oil. To get to the crystalline form the oil needs to be separated out.
Either way, this is fun.
Edymnion
Original Author11 years agolast modified: 9 years agoThat may be what I was seeing as the white skim then, the oil separating out while the cap crystallized. Who knows, but like you said, its fun either way. More fun when you don't know exactly what you're going to end up with, IMO!
DMForcier
11 years agolast modified: 9 years ago> "I'm just sketchy on the legal aspects."
Nothing to worry about. You aren't making the stuff, you're just moving it from one container to the other.
Now if you plan to re-sell it, there might be a issue.
mbellot
11 years agolast modified: 9 years agoNow if you plan to re-sell it, there might be a issue.
I can see it now...
Ghost Pepper White Lightning.
If it don't blind ya it'll burn a hole in ya from mouth to corn hole.
My solids are slowly turning a pale yellow, although I can't say for certain the liquid is really getting any redder or darker.
homefry319
11 years agolast modified: 9 years agonow this is something I may have to try.
have a few superhots going in hydro over the winter may experiment
Edymnion
Original Author11 years agolast modified: 9 years agoJust did my fourth and final pour down.
The mash has become a tapioca brown sludge, and I'd swear the only color left in the alcohol was left over from what liquid was still in the sludge. Either way, I'm calling it. Last batch.
Now the final draw down begins!
Edymnion
Original Author11 years agolast modified: 9 years agoHeh, well I already cleaned out the sludge in the jar, forgot to take pictures of that. And right now its just the same glass of red liquid it was earlier. Still be a couple days before it gets low enough to start being all cool like.
mbellot
11 years agolast modified: 9 years agoAre you artificially warming it?
I was thinking that a heating pad might be just right. Not too hot and easier to deal with than a couple light bulbs inside a cardboard box.
IAmSupernova
11 years agolast modified: 9 years agoWhat happened? I'd imagine it's evaporated by now, what did you end up with?
mbellot
11 years agolast modified: 9 years agoWhat happened? I'd imagine it's evaporated by now, what did you end up with?
Ed spontaneously combusted due to exposure to pure crystallized heat.
DMForcier
11 years agolast modified: 9 years agoHis house, filled ethanol fumes, exploded. Firemen were unable to approach the blazing domicile for over an hour, citing mysterious pepper gas-like fumes that drove them back.
Film at eleven.
maple_grove_gw
11 years agolast modified: 9 years agoSort of reminds me of that Dickens novel where the drunken landlord spontaneously combusted. Anyone remember which one that was?
Edymnion
Original Author11 years agolast modified: 9 years agoI took it off the heat several days ago when it was just about done thinking it would give it time to start crystallizing. Instead, it has gone down to a thick syrup and pretty much stayed that way.
I just now put it back on the heat to see if it'll finish drying it out.
Right now, its pretty much stuck at Aunt Jemima-Went-Straight-To-Hell pancake syrup.
Edymnion
Original Author11 years agolast modified: 9 years agoOh my God, the SMELL off it now is absolutely wretch inducing. Its indescribable.
This crap is going OUTSIDE!
mbellot
11 years agolast modified: 9 years agoEd - I think that's the oleo-resin stage.
I think it's going to require hard science to extract the crystals from that puddle of oil.
smokemaster_2007
11 years agolast modified: 9 years agoFrom the start I've been wondering why anyone would waste so many usable peppers and do the labor to end up with whatever you made.
If you have too many extra peppers,freeze them and then smoke dry them for future use.I also think it would have been faster and easier to make a sohlet extractor.
Use a light bulb for heat and remove the condenser to get rid of the solvent.
Way back when there they sold an ISO 2 for getting essential oils from plant matter.A lot of people made oil by boiling a solvent at low temps in a crock pot with the cover inverted so the solvent dripped from the cover (filled with ice)through the plant material then dripped back into the pot.
To get the solvent out you replaced the plant material with a cup for pure solvent to drip into.Everclear or denatured alcohol were the solvents of choice for their ether like properties but less flamable.
There was an ISO 2
Scroll down for the picture.http://www.420magazine.com/forums/cannabis-edibles/118681-iso-2-oil.html
It was sold as an herbal extractor.
It worked from what I heard.maple_grove_gw
11 years agolast modified: 9 years agoFrom the standpoint of science and engineering, what you're missing is a purification. As a general rule, the purer the compound, the easier it is to crystallize and the converse is just as true: the more impurities are present, the more difficult it will be since impurities will act to increase the solubility of your material of interest.
In your case, your extraction has provided a gimmish of everything in the powder that's ethanol-soluble. It sounds like you'll need to acheive some further purification before the pure cap will crystallize out. Typically this would be done using chromatogtraphy, not something you can easily do at home.
There's no reason why a soxhlet extraction would be any more effect than what you've done, that's simply a way to extract a poorly soluble compound by recycling the solvent. Maybe with a little research you can learn how to purify your extract sufficiently to get it to crystallize, or maybe the crystallization is possible simply under other conditions.
Crystallization is not trivial. Many scientists and engineers devote their careers to it.
Yantz
11 years agolast modified: 9 years agoaccording to this site that sludge you removed was the concentrated capsaicin?
Here is a link that might be useful: Make Pure Capsaicin Crystals
DMForcier
11 years agolast modified: 9 years agoIt says "crystals", but the result is brown liquid.
This sounds onimous:
"Normal latex gloves won't protect your hands from the burning of capsaicin. Heavy amounts of capsaicin will actually melt the latex."
fusion_power
11 years agolast modified: 9 years agoThat is correct. Latex is permeable and will be slightly dissolved by capsaicin. To a lesser degree, vinyl is also permeable but is not readily dissolved.
DarJones
Edymnion
Original Author11 years agolast modified: 9 years agotsheets
11 years agolast modified: 9 years agoI can't imagine trying to clean out that container!! Break out the hazmat suit!! LOL
Edymnion
Original Author11 years agolast modified: 9 years agoActually, after I scrape out all I can I plan to just pour in some more solvent and pour the rest out.
Edymnion
Original Author11 years agolast modified: 9 years agofusion_power
11 years agolast modified: 9 years agoTie that cork in tight. If this genie gets out, there'll be fires from the pit to put out.
DarJones
Edymnion
Original Author11 years agolast modified: 9 years agoI plan on waxing it down once is full. Don't want anything in there getting out. Ever.
rdback
11 years agolast modified: 9 years agoNice bottle! Is it commercially available somewhere?
Oh yeah...nice sludge. Scary, but nice.
Rick
Edymnion
Original Author11 years agolast modified: 9 years agomaple_grove_gw
11 years agolast modified: 9 years agoYou can use it as a weapon if you're ever burglarized :0)
For that matter, here's an excerpt from the Wikipedia entry for "pepper spray":
Pepper spray, also known as OC spray (from "Oleoresin Capsicum"), OC gas, and capsicum spray, is a lachrymatory agent (a chemical compound that irritates the eyes to cause tears, pain, and even temporary blindness) used in policing, riot control, crowd control, and personal self-defense, including defense against dogs and bears.[1][2] Its inflammatory effects cause the eyes to close, taking away vision. This temporary blindness allows officers to more easily restrain subjects and permits persons using pepper spray for self-defense an opportunity to escape. Although considered a less-than-lethal agent, it has been deadly in rare cases, and concerns have been raised about a number of deaths where being pepper sprayed may have been a contributing factor.[3]
The active ingredient in pepper spray is capsaicin, which is a chemical derived from the fruit of plants in the Capsicum genus, including chilis. Extraction of oleoresin capsicum from peppers requires capsicum to be finely ground, from which capsaicin is then extracted using an organic solvent such as ethanol. The solvent is then evaporated, and the remaining waxlike resin is the oleoresin capsicum. An emulsifier such as propylene glycol is used to suspend the OC in water, and pressurized to make it aerosol in pepper spray. The high performance liquid chromatography (HPLC) method is used to measure the amount of capsaicin and major capsaicinoids within pepper sprays.
It's basically your procedure up to aeresolization. Sounds like dangerous stuff there.
Here is a link that might be useful: Pepper spray
maple_grove_gw