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Dragon's Tail
12-20-2017, 08:36 PM
Hey guys, so Dragon's Tail here, still up to my usual chemical/chymical studies, and wanted to share this.

Let me start off by saying that black pepper is amazing:
https://www.omicsonline.org/scientific-reports/2155-9600-SR172.pdf

Some of what I'm going to be discussing references that paper, and if you are looking for medicinal/health effects, they're all in there plain as day.

So, the standard alcohol tincture isn't my end game here, but while bubbling some essential oils out of about 200mL of ground black pepper (which is apparently going to take a while with my current process) I decided to make a tincture with the stuff also, the results: wonderful, penetrating. I wouldn't go more than 5 drops per cup as there doesn't appear to be a need. I used three this morning and I feel less inclined to smoke, more energetic, and in general very good, and I doubt it's because I stayed up all last night drinking, so there's something to this tincture.

Now. I capped away the tincture in 2-30mL bottles and had some left over (I only made about 100mL most). I wasn't sure if there was enough, so I didn't bother with another dropper bottle, but I noticed this white misty stuff on my pouring glass after all the filtering an filling. I added a couple drops of water, and bazinga. The tincture was around 70% alc because the crushed pepper used was already beyond dry, and I wanted to give it a bit of water.

Adding distilled water to the finished tincture precipitated something, piperine, I'm sure of it. Those lousy chemists on youtube are a bunch of tards. When you add water straight to the tincture, the precipitate will drop, and the remaining tincture will float on top. Once it all turns into yellow milk, set it to the side to crystallize. 30 seconds in the microwave or any other gentle heating seems to aide the crystallization process.

I filtered the slurry to get a very bright sulfur looking powder, which is strongly aromatic. Basically, concentrating the best parts of black pepper is SUPER easy and can be done in any kitchen. You don't need sodium hydroxide this or that, and if you are distilling the solvent off, then all you need is more pepper.

I'm currently trying to wash and recrystallize the powder with a little distilled water. Now, the science and safety notes:

Black pepper contains from up to 5-10% of this stuff by weight, so just assume that it's going to be 20 times more potent than your pepper, potentially 100 times if you have crappy pepper. Think about that before sprinkling on your potatoes.

There is another chemical, Palmitic Acid, which is about 1% in dried peppers that also has similar properties to piperine, but it makes a white crystal. The brightness of this first product I have described could be from a concentration of the acid anywhere from 10-50% of the powder.

The reason these drop out of solution is solubility, so definitely not an alchemical property, anyone can do it. They are both fairly soluble in alcohol, and they hate water. My initial eyeball measurements suggest that you get the most yield (so far) between 15% and 25% ABV alcohol, though it might be lower. You will know when you've added enough, just don't shake or stir the mix till it all goes over to milky. The powder at this stage appears super pure and started making tiny crystals on its own after more drying, so like I said, silly chemists and their 12 step process :D

While Palmitic acid appears naturally here, and the pros/cons are up for debate, I can't see this being worse in this form than in the natural product, but I'm looking for ways to get rid of it. It is MUCH less soluble (about 50x less at STP) in water than piperine, so washing through filter paper and recrystalizing should pretty well rid you of any trace amounts, just like we do with plant salts. It also has a lower melting point (63C vs 130C). Might even be worth hanging onto some, if it's actually in the yellow powder at all. It's slightly more soluble in alcohol so it might still be in the leftover tincture solution. I'll let you know if I end up recovering any. This is just a friendly warning about a potential impurity, it may not show up.

While your yield will be a little lower than the long way, for sure, this is a safe, easy method, and the drop in product is minimal, especially when comparing the cost of NaOH vs just getting more pepper. :P

Aham
12-20-2017, 09:52 PM
Good work DT! Did you get to use any of your new glass? :)

Dragon's Tail
12-20-2017, 10:03 PM
Good work DT! Did you get to use any of your new glass? :)

The new flat bottom 250mLs are very handy :) I also used my straight take-off adapter to make a sort of buchner funnel when I was filtering the powder. My distillation train at the moment is using old parts, but I'm going to change it up to a retort type setup for the next batch of fluid. 200mL of black pepper ended up making about 1.5L of decoction and I was worried about overheating. Think I have it under control now I need to get the thermometer into the water to keep an eye on it instead of sticking out of the sand bath, so I will probably use the new claisen and elbow on the next run with my single neck boiler. The 500 is a bit too small for this and I'm not sure what kind of sticky will come out. Don't want to stain the brand new bottle just yet.

Aham
12-20-2017, 10:15 PM
Sounds like you have most of the mechanics worked out. :)

Pics of the process would be nice.

Dragon's Tail
12-20-2017, 10:52 PM
As far as THAT process. I want to get a little farther along. I was thinking of cooking pots, pretending to be an ancient watching the stew boil and the veggies get mush, wondering what would happen (or likely did happen a lot) with just letting it boil in the pot all night.

Flash back to reality, I tossed some pepper and water in a 1L boiler and put a reflux on it for a couple days, nothing popped into the collection flask way up top. I kept trying to water down the solution because I feared it would scorch, but that didn't help anything except make more. Just trying to tease the essential oil off gently now.
this little cave forming was pretty cool. The first batch, 200mL of pepper drank every bit of 400mL of distilled water:
https://i.imgur.com/QlHAg5S.jpg

On the tincture side, I did manage to snap a shot before the last bit of water was added to make the milk.
https://i.imgur.com/VmkZo1m.jpg

I tried this with some other tinctures and it (obviously) didn't work, no similar compounds. Closest I got was slightly cloudy. The tincture process above is pretty straightforward. Tincture, decant, filter, store whatever tincture you want to keep, and then titrate water until the milk curdles, hehe. I didn't dry off the eth solvent first, which is the first step of the chemical separation. My way is much easier, and likely a purer product. I don't know why the chemists do that long involved procedure.

elixirmixer
12-21-2017, 09:32 AM
Can we see the crystals DT?

Dragon's Tail
12-21-2017, 02:28 PM
Can we see the crystals DT?

They're still drying, they look like yellow powder mostly, except the tiny ones on the wall of the glass. Once I collect the rest and dry everything up, I'll snap a pic for you guys. If you're lucky I'll break out the macro lens. Piperine crystals are cool looking but all the pictures online show them tiny.

elixirmixer
12-21-2017, 10:13 PM
Oh and yes I do happen to have a black pepper batch sitting in absolute alcohol.

What do you want me to do with it?

Dragon's Tail
12-21-2017, 11:57 PM
EM: Basically wondering if you get the same results. It doesn't take much to test. I used a 70% alcohol concentration, but should still work with absolute. If you take around 20-30mL, add distilled water. You can do a drop at a time at first, and you should see a titration type of reaction with a white cloud appearing and then rendering away immediately. If you add a bit more, the cloudy layer will separate to the bottom. I think about 4-5 parts water to one part tincture should do the trick to precipitate as much piperine solution as possible. It has to settle for a couple days, but it will clump up, and then you can filter it off. Let dry and make your own crystals, haha.

Update. I noticed in the filtrate some streaks of green, so this might be the tar dropping out after a bit of drying. I also started thinking, there will probably be some waxes/oils too. My little crystals are starting to form, but they're tiny, spiny, and a bit cloudy. After all the solution dries I'll post a pic. It's evaporating in a warm spot next to my distillation pot.

elixirmixer
12-22-2017, 08:43 AM
I will happily put my full batch to experiment with this process. That's why I love you DT because your always looking at spagyrics from an almost completely opposite view to me, lots to learn by studying your works.

I can almost guarantee the same result as most alcohol extractions, when water is added, your other non-precipitating tinture is the anomaly.

However, I never saw value in the precipitate, which you have kindly pointed out is foolishness. So thank you.

Camomile, frankincense, rosemary are three off the top of my head that I know drop precipitate when water is added.

This shit is the result of using alcohol.

Its better to use the existing moisture of the plant and not use alcohol at all in my opinion, however this takes either very expensive set up, or shitloads of patience...

elixirmixer
12-22-2017, 08:46 AM
I recommend your next tincture to be tumeric. Black pepper and tumeric have a symbiotic relationship in the body of causing serious antiinflammatory effects.

I've helped people with serious sporting injuries with these two bad boys :)

Dragon's Tail
12-22-2017, 10:01 PM
I recommend your next tincture to be tumeric. Black pepper and tumeric have a symbiotic relationship in the body of causing serious antiinflammatory effects.

I've helped people with serious sporting injuries with these two bad boys :)

It was on my mind. Also agree with alcohol being more of a distraction to the alchemical preparation of plants than anything else. The more I learn, the more I'm thinking that the long boring chapters of "philosophically" preparing spirit of wine is bunk, and that the solvent needed is actually prepared from water and some distillation methods to make it "different" from common water. I've had water that resembles what they call "burnt wine." Looks like ordinary water, but is oderous after overcooking with plant matter while distilling. It will also burn your mouth if you drop a teaspoon or so on your tongue and hold it there for a second. You already know about my "golden" water from distilling saline solutions. I'm going to give Hollandus another read one day with this in mind. My "big" pepper experiment is actually being done with just distilled water and pepper. Nothing else added (cept maybe a little dust from the air). I don't have any results yet. I'm trying to cook off as much of the oil as possible, and then I will filter and dry my gums/resins. Also saving the "spent" plant matter for further experimentation before I burn it up. I'm making plenty of hydrosol this way so far, but not too much oil. There should be about 5% by weight essential oil that doesn't degrade up to 140C, if the chemists are to be trusted. The tiny bit of gum that I got from the alcohol tincture is wetter and stickier than normal, but also smells of wonderful pepper aroma. We'll see if the same is true for the water extracts.

Dragon's Tail
12-22-2017, 10:16 PM
Okay, here are the crystal pictures:

https://i.imgur.com/qonZVFd.jpg
https://i.imgur.com/o5oFso1.jpg

The first photo is one of the clumps, what you will see on close inspection with a small magnifier.
The second is a macro shot of a big clump attached to the one in the first picture, so you can see the tiny crystals clearly. The longest one I found is about 2mm x 0.5mm, give or take, and it has a red tip.

There wasn't much here. As I said, about 20-40mL of tincture to make this. I weighed out about 3 grains. Might as well put the math here for reference...

Piperine will go to ~66g/L in alcohol, so 10mL should have a little over 1/2 a gram, or about 8 grains. Obviously I had more losses than I thought, but the filtered solution was still VERY yellow. I'm sure some of it is getting bound up in the gum, and about half of the original filtrate is still soaking in the water I cleaned it with. Still, pepper is cheap, and this extraction method can be done without ANY apparatus except a couple bottles and some filter paper, so I think for someone new to spagyrics and synthesis of compounds, it's a very nice experiment.

Conventionally these are washed and recrystallized in acetone. Again, screw that. I don't trust the stuff at the store, and I'm not distilling my own. At the risk of major losses, my Next trick is going to be a couple parts. The crystals will be put into a filter, and washed VERY gently with water to remove soluble compounds. I'll toss this water, and then dissolve the rest in absolute, and then allow to dry and recrystallize. The result should be fairly pure, I think. Hope you liked the photos,

-DT

Schmuldvich
12-22-2017, 10:30 PM
Beautiful!!

What do you do with the crystals?

How stable are they?

What is the medical dosage?

Dragon's Tail
12-22-2017, 10:49 PM
I can almost guarantee the same result as most alcohol extractions, when water is added, your other non-precipitating tinture is the anomaly.

However, I never saw value in the precipitate, which you have kindly pointed out is foolishness. So thank you.


Interesting. I believe I tried a dead nettle extraction, which got slightly cloudy, but nothing like what I saw here, even with copious amounts of water (mixed up a tiny bit in a shot glass, then filled it the rest of the way with water). I have some other tinctures laying around that I'll experiment with. Could be interesting, especially if they will clump into filterable crystals after 24-48 hours. Could be interesting to figure out which compounds will exhibit this kind of behavior, or if there's any correlation between plant types. Rosemary and Frankincense for sure, I would consider "hot" herbs, chamomile not so much. (Frankincense isn't an herb but you know what I mean). Hmm, lots to think about, and perhaps there is a meaning to the ability to make a tincture that will "irish car bomb" when you add water to it. This method of coagulation is interesting to me for sure.

Dragon's Tail
12-22-2017, 10:59 PM
Schmuldvich, they should melt around 130C, so I expect that they are pretty stable. They don't appear to be delequescent. As far as dosage, I'm not sure what the LD50 is, but 3-5 drops of the tincture in a cup of water makes it VERY peppery and exhibits some effects. 1mL of pepper tincture could contain a MAX of one grain of this stuff, so it's super duper concentrated in the solid form. I think there are strong doses used as a test cancer treatment, but in general, I don't think more than a gram per day would be wise, and certainly not all at once, even though I think the anecdotal "cancer" thing was around 50 grams.

Also, since the precipitate will dry with the natural gums and oils of the peppercorn included, I think that would be better for a medicine. It's almost reminiscent of a "nature made" stone of black pepper. Perhaps moreso with the addition of a little tartar salt ;) I'm refining my little batch just to see what kind of crystals I get, and I might add some to my final preparation, or just make a bunch more :) It's very cool stuff. Good for treating high blood pressure and anti-inflimation, as EM mentioned, and all the other things on the linked PDF, but the biggest thing with this is making other things more bio-available. I think that mixed with other tinctures or as an ingredient in a more complex potion, this could enhance the effects and strengthen other medicines.

elixirmixer
12-23-2017, 09:05 PM
Could you dry distill those crystals? Or volatize them?

Dragon's Tail
12-24-2017, 03:33 AM
If I had to guess, from the proposed chemical structure, dry distillation might be possible. But I'm not ready for that yet. I need to get my lab setup at the property where I can get more experimental. It's an aromatic compound with a carbon ring, so I suppose dry distillation is possible, but I'm guessing.

I don't think they are volatile alone, however an acid salt can be made from them by hydrolyzing, and that might go over the still head. Not sure. Interesting thought though. I have no real plans with the crystals, as I'm working on low temp cooking of the plant matter in water to get my materials for a jelly ball. So far it seems to be going well, but I still have a long way to go. I'm at around 500mL of hydrosol and a tiny bit of oil, the leftovers are turning themselves into powder after decanting off of the raw ingredient. The pot that I have going right now has been distilling for a day and a half, and I still have another repetition to do before I separate the first waters from the ground pepper. Then I will probably add the hydrosol back to the feces and distill again, separating off the powdery residue as I go. I'm trying to keep some notes so that I can do a decent write up later if anything interesting happens. The crystals were a side project that I thought would be cool.

My brother used a few drops of the tincture in his soup tonight, after battling with a cold. He thought the immediate crystal formation was neat when the drops hit the hot water. We haven't discussed it, but he's up and animated now, obviously feeling better. It's great stuff, and so easy to prepare. The tincture alone is, I think, worth the time to add to any medicine chest.

elixirmixer
12-24-2017, 03:44 AM
So the crystals and tincture are separate things? Is the tincture just black pepper boiled in alcohol and filtered out the crystals?

Dragon's Tail
12-24-2017, 03:56 AM
The crystals came out of the tincture by preparation. But the tincture was a side project while my actual experiment with water is ongoing. The crystals were a nice surprise :)

So, I'm keeping some tincture for a gentle medicine, and making another batch that I will try to get more crystals out of for a concentrated preparation. But the experiment to make the spagyric preparation is being done with water rather than eth.

elixirmixer
12-24-2017, 03:56 AM
What do you know DT about the chemical situation associated with this crystal precipitate. Why foes it drop out of solution when water is added? Is this precipitate going to be the same.or different in other plant species?

Do you have any ether? Would be interesting to see if its soluble in ether. Ether seems to be a pretty epic way of doing spagyrics, of coarse it has its disadvantages.

Wife's in the city for Christmas so I'm on daddy duties at the moment but I'll try and get around to distilling some water so I can try this out.

Dragon's Tail
12-24-2017, 04:25 AM
I think it's all about solubility and the alcohol concentration. The chemical in question for crystal formation is piperine. It has a solubility of 66g/L in alcohol and 40mg/L in water. I think diluting the alcohol more than makes up for the difference, so the piperine is forced to precipitate. When dried though, it's going to collect some of the essential oils/waxes/tar/etc dissolved in the tincture, so it won't be super pure. I still have a couple of days on the recrystallization, so far I'm getting clear, icy looking delicate crystals on the walls of the drying glass, but we'll see when they are done. I think they are just to thin on the glass to pick out the color.

I don't have any ether and don't really feel any need to use it at the moment. There's plenty to be discovered in our common waters ;) The water is a mystery of it's own, and I don't think ether was a common solvent for the ancients ;)

elixirmixer
12-24-2017, 04:58 AM
Do I have to steam distill black pepper to get essential oil or can I just boil a pot of blackpepper and condense?

Dragon's Tail
12-24-2017, 05:30 AM
It's usually done by steam distilling the peppercorns. I've boiling black pepper solution and collected some, but I cocked it up a bit. I was so paranoid about burning the herb and getting the temp down that I ended up with lots of hydrosol. I've never really thought the oil to be that essential to the process after meddling with the resins, that's your catalyst for congealing everything, I think.

I'm trying to collect some for the mix, but the hydrosol should provide plenty of food for the stone. I don't know if the ancients concerned themselves with the separated oil so much as following the smell. The other thing is BP soaks up water like a sponge, so if you boil it, you need a high water to crushed pepper ratio. 5:1 at least by volume as I see it, otherwise you'll scorch the material. I haven't worked with water much, so I'm still learning the process. If I can get a system down, I plan on doing more work with mullein next year.

Are you planning to do a similar experiment with water as the solvent?

elixirmixer
12-24-2017, 06:16 AM
No I'm going to make the yellow crystals and then reflux them in either their hydrosol or their essential oil.

If you think they are penetrating now, wait till they are volatized.

Dragon's Tail
12-24-2017, 06:57 AM
No I'm going to make the yellow crystals and then reflux them in either their hydrosol or their essential oil.

If you think they are penetrating now, wait till they are volatized.

sounds like an interesting experiment. Tell me how it turns out. I might be making some more crystals soon, just cause they are so cool, but I'm going to let the washed solution recrystalise first. I might try to specifically go after some black pepper oil and follow your example. I have plenty of hydrosol available at the moment. It would be interesting to follow your progress. Please post pics if you volatize them.

What procedure are you planning? A circulation with the white queen 7 times and then heat gently to tease them to the top of a flask? I still haven't done a proper salt volitization, and I'm suspecting that armoniac has to be captured in some form or another to make it happen chemically. At 130C they should melt, so it might be trickier than volatizing tarter salts.

elixirmixer
12-24-2017, 07:24 AM
To my knowledge your yellow crystals ARE "Our" Sal Ammoniac.

Salt of Sulfur. I believe these are easier to volatize than potash due to their aromatic nature.

It will take some time because the lab is a mess. I'll have to wait for my wife to come home to do the full experiment, however I'm going to have a nap and begin working the black peps.

You've re-engaged me in spagyrics with this one as I always looked at the water separation as a FAIL. Hoerver, I didn't realize that drying the precipitate resulted in beautiful crystals. Are they flammable?

I have proven salt volatilization in the lab using hydrosol but only as a proof of theory I didn't continue with the circulation's and didn't build up a collectable yeild.

I believe in this case that essential oils are preferable for tartar, and that the hydrosol is to be used on the yellow crystals. Earth + Air / Fire + Water. Tartar + aromatics / pigments (piperine) + waters (hydrosol).

This is my understanding. Let's see how we go anyway.

Once again, always a pleasure working with you DT

Dragon's Tail
12-24-2017, 03:57 PM
Cool beans. You may be onto something with the crystals having their own special place already. The hydrosol is carrying the oil (volatile) and the crystals definitely give off a scent of the flavor compounds. I'm really interested to see your results and specifics about the process if you are willing to share.

Ripping the pepper apart through long slow distillation (water as the solvent) hasn't yet dropped any of the tars, and a powder is falling out of the solution slowly, so even the simple aspect of extracting the bitumous matter looks like it's going to be a couple steps of gravity filtration. Will be interesting to see if the piperine comes out of the sediment, or better if the resin produced is characteristic of piperine by the water method. This is one reason I started the tincture in tandem with my water extraction, so I would have notes to compare with. It'll be another week (at least) until I can ascertain if the water extraction also precipitates piperine from solution with the other tarry elements. Once that's done I'm going to try extracting more from the leftover earth, as it's still quite dark, this time with the hydrosol.

elixirmixer
12-24-2017, 10:16 PM
I believe right now DT you and I are working on a completely new way to perform spagyrics.

Cool ey.

Dragon's Tail
12-25-2017, 02:58 AM
I believe right now DT you and I are working on a completely new way to perform spagyrics.

Cool ey.

Somebody's gotta do it, lol. And using 2 different processes at the moment. Hopefully when we compare notes, we'll make some new discoveries. I'm keeping with this water process for a minute, because I've had my mind set on it for a long time. I think our goals for spagyrics are in line--make good medicines. Little rocks are cool, but what good is it if it doesn't work? I also believe that the ancients were following the medicine path, and that led them to magestries and stones. Working backwards from the end product seems a little silly. I learn more by trying stuff, and then note interesting correlations with the texts.

elixirmixer
12-25-2017, 03:49 AM
Well I've certainly learnt alot about pepper. This piperine is really quite amazing (our little yellow pepper precipitate for those who have just joined us) in that it basically 'occupies' the liver, allowing other "drugs?" to reach higher levels within the blood. Basically; by using piperine we get more effect out of some of our other medications.

As an example, curcumin (found in tumeric). The liver effectively eliminates curcumin very quickly out of your blood, however, using in unison with piperine, reaches MUCH higher levels than it would otherwise.

elixirmixer
12-25-2017, 03:57 AM
Also FAT does something good with the curcumin too. Forgot what it was now but a nice pepper, fatty curry is a good way to go.

elixirmixer
12-25-2017, 09:51 AM
DT you are really on to something here and so am I now.

I'm pretty sure curcumin, piperine's best friend is extracted in almost the exact same way. I also have some tumeric tinture so I will give this a go and see.

elixirmixer
12-25-2017, 10:32 AM
Yes. Curcumin just dropped out of solution. Do I need to be careful with how much water I add? I kind of just hosed down the pepper till it all went white and now I've got it on the stove for a bit. Should it get a bit gluggy or something when its ready for filtering?

I'm not sure how much water to use so maybe I'll just use enough that half the solution precipitates on the tumeric.

This method is quite golden really. Its a further way to purify an alcoholic tincture and separate things that are non water soluble. Its allowing us to isolate certain beneficial salts such as we are doing here. And, it allows someone like myself who utilizes different methods to basically RAMP up other alchemical preparations by adding the key ingredients if those happen to be the non-water soluble components. Definitely could help give a stone both the kick to be effective and that beautiful crystalline structure to look nice and appealing.

Your little marble stones look interesting, however I'm looking for nice crystals that can be cast into beautiful shapes. Shapes that will correspond with the planetary sphere of that plant. But that's just to look pretty really.

elixirmixer
12-25-2017, 11:26 AM
Pinine can be extracted using this method from rosemary, sage and pine sap.

Pinine is used in traditional Chinese medicine as an anti cancer tool and there have been studies that suggested a 40% reduction in melanoma in mice.

A very simple process and yet look at everything we can do with it!! Well done DT!! This one has to go into the Spagyrics book!!

Edit: also, I think you were right about adding a little heat to the black pepper water-alco tincture. My tincture was a more green rather than yellow but the heat really brought out the yellow colour of the piperine. I've put it in the fridge now to help drop out more precipitate. I did about a 2 part water to 1 part tincture. I don't want too much water because then I'll dissolve some piperine and other shit I don't want.

elixirmixer
12-25-2017, 11:45 AM
One final thing. If tumeric essential oil is added (sesquiterpenoids) then the bioavailability of curcumin is greatly enhanced again. This is some serious fire power when trying to solve serious issues such as rhumetoid arthritis for example.

Dragon's Tail
12-25-2017, 01:53 PM
Sweet, nice to know about bombing tumeric and pine. I'm trying to dry some of this spent pepper at the moment, and it's being fussy. Been at 90C all night and it's still jelly, hehe. Well, there's some crunchy bits too.

On water, I basically added all I needed until the tincture went "all cloud," like that picture on the first page is basically just before the final splash of water. It really needs to coagulate a little before filtering because the particles are so small, I think they pass right through coffee filters. I did this by setting up for 24-48 hours and letting them crystallize a bit further where they could get trapped.

Still waiting on my recrystallization to dry. I added a tiny piece for nucleation and it didn't dissolve, so hopefully we'll be seeing them soon. I hope. The solution is almost gone, lol. I've got some more cedar, it's a hot herb too. I'm not sure if it had salts added to it or not, but I'll try water bombing some of it later to see if it acts like it's evergreen bretheren. What kind of sage are you using? You have a latin name for that one by chance? There's all kinds of unrelated "sages" out there, especially in common speake.

Dragon's Tail
12-25-2017, 02:27 PM
yep, add Red Cedar (Juniperus Virginiana) to the list. I had a completed "spagyric" (just tincture plus leeched salts) laying in the back of my cabinet. Adding the salts drops a red mist that coats the bottom of the glass, this I new. Even so, the tincure still bombs. about 1:1 water was added. Cool.

The only "ingredients" I can find about cedar at the moment are components of the essential oil, so that might not be what I'm seeing. It has a light coffee color. I'll dig into the pine component later and see if it's is the same thing that you found there.

elixirmixer
12-25-2017, 10:58 PM
Just putting my piperine down to dry now. I actually filtered it before the partial size grew and now it looks like I'll be getting some pretty pure crystals. Lovely colour. Its surprising what a little warmth can do some times.

Dragon's Tail
12-26-2017, 01:05 AM
Do you think the heat helped to coagulate it a little bit? So far, for me these tincture bombs look like emulsions. I was actually surprised that I could filter the solution at all the first time (after letting it stand at room temp), and a lot of milky yellow still passed through even a double coffee filter.

elixirmixer
12-26-2017, 02:16 AM
It's really hard to tell completely what's going on here. I'm just waiting on drying to see whether I'm getting crystals or just a brown stain.

elixirmixer
12-26-2017, 09:46 AM
So.... I failed. I'm not sure what went wrong but I didn't get any piperine. I thought I was going to get it, the colour looked right but it all evaporated into basically nothing. No idea what I did wrong. Maybe I should have left it longer to clump up as you did.

Ill try again but I'm scared of failure. I get so depressed when lab stuff goes to shit lol.

Dragon's Tail
12-26-2017, 03:52 PM
So.... I failed. I'm not sure what went wrong but I didn't get any piperine. I thought I was going to get it, the colour looked right but it all evaporated into basically nothing. No idea what I did wrong. Maybe I should have left it longer to clump up as you did.

Ill try again but I'm scared of failure. I get so depressed when lab stuff goes to shit lol.

I'll have to read over your notes again when I get some time later. I collected the piperine first by catching it in a filter (after sitting for two days). I wasn't going to allow that long for the cedar sample. I just did a couple CCs to see if it milked up. You might need more water, but you should definitely notice it start to settle and separate on it's own before filtering, otherwise the particles will probably be too small and pass through the filter (unless you have one of those fritted glass things. I don't). I washed it further from there instead of trying to purify straight out of the box.

My rectified piperine is starting to crystallize nicely (after frickin days) but there's still a couple mL of alc solvent in the glass, so I'm going to let it go till it's done. I have a pretty good little crystal going on it from the clump, almost a mm in diameter.

Extraction of the cloud from the solution is something I plan to look into further. I'm brewing up about 200mL of tincture by adding a little pepper to it at a time and letting it sit for days, with shaking, until it goes dark. Hopefully I can get a gram or two out. Since I'm purifying with alc it might be interesting to distill off the alm/Mercury, redissolve the separated piperine in that, and they dry to get the crystals while at the same time collecting the black Sulphur. The water extraction is still my focus though.

elixirmixer
12-26-2017, 09:10 PM
I'm going to give it another go. I seriously cannot comprehend where the piperine went!! Could it possible volatize with the alcohol?

No idea but I'm so pissed that I have to try it again. I will take it slower And allow for clumping and settling as you suggest. The curcumin came out okay. Its not a crystal but a powder. I had a mad tumeric and pepper rice yesterday and it did wonders. I was suffering from inflamed gallstones which really hurt and rverytime I eat something made them worse, but then I ate the rice thinking that it could hurt or it might take down the inflammation and lo' and behold, fixed me right up. Go piperine!!

Dragon's Tail
12-26-2017, 09:29 PM
Right on. Just wanted to make sure that I let you know the piper was in fact filtered off, and it looks like kind of a shaggy powder until you look at it real close. The original crystals were super tiny, like little hairs. I just blew them up so they could be seen better. When I get the big batch going I might see if there is something I can do to tease them out, like maybe distilling off the eth from the solution or just popping the mixture in the fridge for the night.

After what you said, I definitely believe that you have to get the piperine away from the solution first before you try to do anything with it. When I redisolved in eth it took a lot of stirring and it didn't want to get ate up in solution, but then half of the new mixture had to evaporate before I put put a crystal seed in without having it completely dissolve a couple hours later.

The recrystallization is going well. I dropped the orange/yellow clump in a filter paper and eyedroppered a couple CCs distilled water over it. Just enough to soak the pile and drive off any water solubles. Then transferred to a shot glass and added a little eth, swish around, repeat, until most of the solid dissolved. The transferred the new dissolved piperine to this glass and let the eth evaporate off over the last few days, nice and slow. This is the result:

https://i.imgur.com/UCe7RYg.jpg

The crystals are much larger and visible without squinting. They can probably get bigger if I had more material, but they are quite pretty. I'm going to dry a couple and then add some heat to watch them melt, which should happen with a minimal amount of heat from my torch under a spoon or something. They're supposed to melt at 129C according to the report I read about the typical chemical extraction/synthesis, so melting into a little pool of waxy will confirm that this is indeed piperine, as there isn't much else it could be at this point.

Dragon's Tail
12-26-2017, 09:50 PM
That was cool. I took one of the little crystals and heated it. It melts like ice, going straight to runny and started to boil. I think it decomposed because it solidified as a gum/resin, which I scraped off the spoon with a knife and rolled into a tiny yellow bead with my fingers. I don't think it's a good idea to flux this one.

elixirmixer
12-26-2017, 10:09 PM
Yes there is no boiling point, only decomposition, and yes, those crystals your growing certainly look exactly like what piperine should look like so I would call that quite a success.

I understand how you went about it, I just tryed it slightly differently with complete failure so this time I will stick to the plan and see how we go.

Because I suffer from gall stones and because this really does the trick, its in my best interest to master this one.

Did you at any stage evaporate off your alcohols or did you simply, add water, allow to clump, then filter. Did you put it in the fridge? How long should heating be do you think? I had mine on a good heat but not enough to boil for about an hour or so, I'm thinking this may be a bit too much. I might skip heating all together and just be much more patient, wait for clumping ect.

I wish I was a better chemist. If I fail again it will break me lol

Dragon's Tail
12-26-2017, 11:19 PM
I didn't do any special preparation for the clumps in the original images. The tincture was done in a dark place for about 5 days with 70% eth alcohol (grain alcohol diluted with distilled water). Water was added to make it milky, and I believe the "milk" sat for about 48 hours before filtering through coffee filters. I collected the mass in the paper, and that was fairly pure piperine with some oil and I believe a little of the gum mixed in. The recrystallization took even longer, and if I had to guess, halfed the yield. I'll weigh them when they dry off all the way, even though I already swiped a couple of the smaller crystals, just to see how much I lost through purification/recrystallization in alcohol.

I think an absolute alcohol will work fine. If I figure out how to clump everything better, I'll post it.

elixirmixer
12-26-2017, 11:31 PM
Okay let's get this straight though, you used about a 4 parts water 1 part tincture? Is that right?

Dragon's Tail
12-26-2017, 11:42 PM
Okay let's get this straight though, you used about a 4 parts water 1 part tincture? Is that right?

Pretty sure that's how it went down. I didn't measure beforehand. Just added water slowly, letting the milk settle under the remaining tincture. All the light solution sank under the alcoholic tincture, and I added until the tincture layer disappeared. Guessing from looking at it, I suspect 4:1 or 5:1.

Dragon's Tail
12-27-2017, 02:55 PM
2.2 grains recovered from the initial ~3. Guess I should have been more precise. Still, for such a tiny amount, that isn't much loss at all. Some darkness precipitated after everything else dropped out, so there is still a touch of gum in the sample, but the crystals are there. I just put one in my monster, and funny enough I can't taste it yet. Perhaps it'll take a minute to solve, but I have a feeling that the pure piperine is more subtle, yet it contains all the heat compounds, so it's not to be underestimated. I think I can feel the heat in the back of my throat. Or maybe that tiny half-crystal was too low a dose, but knowing how potent the tincture was, I'm not going to be brave and eat the whole clump, hehe.

On my water extraction, I left some salts curing on heat for about a day. They weren't quite white, but offwhite, with some carbon still about. Solved in ~200mL of the hydrosol, and the "not unpleasant" smell that I'm becoming familiar with rose from the mixture. I filtered and it's milky. I think I will be distilling off the "water" rather than heat drying, but that's going to be a process, so I'm trying currently to extract my honey/gum from the remaining fluid, if there is any to be had.

I couldn't help thinking that the salt mixture has all the normal "elements" combined, my Mercury being water, the essential Sulphur bound in a matrix of water as a hydrosol, and the salt, which has brought out the white coloring of the thing. It will be interesting to "balance" those elements through distillation, but I may repeat several times. When you guys are volitizing salts in this way, do you distill them to dryness and then sublimate by upping the temp, or do they start going over the still head with the "water"?

Dragon's Tail
12-28-2017, 07:21 PM
Okay, officially switching gears. I'll condense my notes about the whole "water extraction" process later on. Just wanted to see if this rang a bell with anyone.

Aside from the classic tincture, my new spagyric concoction is made with just water and black pepper, at least that's the intent. I'm essentially drying the cleaned up decoction of the pepper in an open top jar. This should be relatively free of oil and the precipitates have dropped from it through several distillations to get most of the original solvent out first. The smell of the cooked liquid was similar to the brine that I boil peanuts in, but once it began to dry and started making a cloudy layer on top, it took on a sweetness. It's now very thick, almost dry honey, and a skin has solidified on the surface. The interesting thing though, is that it's making these wrinkles around the outer edge, which are in motion. So it will wrinkle up for a second, and then smooth out. Could probably explain it with convection currents or something, but it's cool to watch. I'm debating whether to remove the skin, and transfer the honey that hasn't yet dried to a gum, or keep going until it all thickens. There wasn't much actual gum out of the whole process, so a smaller vessel might be better for it. This should be my bitumus matter for the magestry. All in all, making progress with doing everything with water, and that opens the door to many kinds of solvents besides eth alcohol for plant work, and my results continue to be awesome. We'll see what kind of end product I get. Next steps are separating the precipitates from the extraction and figuring out how to purify those, checking if they are piperine. I'll also be cohabating the salt/hydrosol solution to purify the extract from the ashes, and I've saved the calcium carb stuff caught in the first filtering. Quite a few products from the original decoction. Now to figure out how to recombine them, looking for a sign.

Dragon's Tail
12-30-2017, 05:18 AM
So my distillate from the salts did a couple of things. First, it refuses to boil. I finally turned the temp down and covered everything in tinfoil up to the neck with the 70deg elbow.

The distillate is interesting. It's crystal clear, but smelled burnt, so I put it in a bottle with some other "burnt" water that I caught earlier, but when I came back today, the campfire smell was gone and it smelled very strongly of the pepper. Maybe the nose screwed up before, but I think a little time to cool down and do some degassing maybe works off the fire smell, or it ripens. Perhaps the salts work to fix the aromatic elements where they can fuse properly with the water?

The salts themselves colored the hydrosol a faint yellow, and some yellow skin has evolved, even before the salts themselves precipitated. I dropped the rest of the solution in a crucible to dry off the rest of the way, leaving the yellow film on the walls while the crystals collected in the bottom. It isn't much, but I have more material to calcine that's just sitting around. Trying to take my time and figure out each step of the process slowly and carefully. So the next step for the salt is to calcine again, and pour on about half of the "fire water" mentioned above that came out of the original solution. Also of note. Some of the salt dropped out of the cold solution before I distilled it, but there was no sediment at all that I noticed after heating started.

As far as the concentrated extract from the last post. I skimmed the skin off the top, which looked kind of silvery against the black/red fluid, and poured the liquid part into another dish to cool. It was a little thick over heat, but it's pure jelly on cooling, and retained the sweet smell. I'm also noticing that sweetness in the precipitate from the extract. The precipitate is kind of a bitch, because it's so liquidy that it can't be dug out with a spoon, yet big enough particles to instantly clog a coffee filter. A fritted filter might be handy but I can't be fucked with the expense at the moment. I did manage to collect some, so it's drying, and it has that sweet smell to it. Carbohydrates maybe? The jelly is sweet, but the black liquid part of the extract has the pepper smell (which might be what I'm finding in the watery distillate).

All in all. I feel like I'm learning a lot. I'm trying new things. Reading over more texts, and confident that whatever I concoct will be a wonderful magistry. The Tincture alone is quite strong. I took five drops this evening and it was too much in about 3 oz of water. Like pepper times 100. The water extract project is much milder on the tongue, but I can feel more of a spiritual effect as I continue to experiment with it, at least as strong as the tincture. But if you want to have some pepper flavoring for your food, just saying, tincture all the way. It's f'cking amazing!

I'm doing a first attempt at purifying a tiny amount of the gum from the leftovers in the glass I poured it off from. I have some suspicions that cohabation, when understood properly, will render purity to the "stinking black mass," If it works, I may try it this way on the next alcohol tarry extract. IMO the tar/resin/gum contains the best medicine, and learning to work with it has been a mystery for me, and maybe it's harder with alcohol work, but I'm going to keep trying at this until I figure it out. Last ditch will be combining with the salt to try and bleed it, but that's still a ways off.

elixirmixer
12-30-2017, 08:44 AM
Keep it up. I'm still digesting a new batch of black pepper in alcohol.

Dragon's Tail
12-30-2017, 02:18 PM
Keep it up. I'm still digesting a new batch of black pepper in alcohol.

Let us know how it turns out. Getting that misty stuff away from the water fraction is almost always a pain in the butt. I have another "cloudy water" thats being fussy. Pressurised filtration seems to help, but I have a regular funnel, so I drop it in a straight tube with a thin plastic film to seal the connection, link the tube to a take-off adapter and then a flask at the bottom. Connect hose to pressure pump (in my case my lungs so I have to be careful with strong solvents, even alcohol). I might put a buchner funnel on my list soon.

Dragon's Tail
12-31-2017, 08:58 PM
So, the Sulphur extracted with distilled water was originally evaporated off with some heat, skin was removed, and the black/red/orange liquor was poured off and gelled. After some insight gleaned from the leftover crusts, I resoaked the jelly, both with original hydrosol and "burnt" water distilled off the purifying salts. Both mixtures took on the same smell, and reacted similarly, precipitating some white/gray mass (which turned black and hard on drying) which was filtered off. I combined the two (since they looked/smelled/seemed exactly the same) and am evaporating at 60C. This little crystal showed up swimming on top. The first drying produced a cloudy mist and a skin, so far on this one, only this crystal and a little sunken cloudy. All other white areas of the picture are reflected light. Up close, it looks like a tiny feather rather than a single crystal point as it appears here.

https://i.imgur.com/1RRXMBx.jpg

I still have about half of the jelly separate, and it seems to be bleeding a tiny amount of red fluid. I only noticed because I was thinking about making an alcohol tincture of it similar to the ens process. Still undecided on that, curious to see what happens as it continues to sit in the dark in a stoppered bottle.

Dragon's Tail
01-01-2018, 12:56 AM
This is the "Salt of Sulphur" from the test batch of leftovers. When they coat on the glass they are a translucent yellow. After scraping them out they are dull read but full of glittery sparkles...can I say "glittery" without my man card being revoked?

https://i.imgur.com/lvyAIA5.jpg

My primary Sulphur for this project has not taken on a solid phase yet, just liquid solution on goop. Gotta make sure I get all the crap out before I dry it. I filtered some of the cloudiness while it was hot. I might filter again before this drying phase is done. Coagulating with water dropped some where it could be filtered, but I might have to repeat the process, oh, I dunno, six more times? ;)

My plan is to unite these S Salts with the plant salt, dissolve in the hydrosol water, chill it for a bit, then evaporate together. Plant salts are on their second distillation/recrystallization.

elixirmixer
01-01-2018, 02:08 AM
I'm hoping that during these experiments you learn more about the piperine extraction and share how I am to proceed without failure. I have another tincture prepared.

PS: nice glitters

Dragon's Tail
01-01-2018, 04:22 AM
I'm hoping that during these experiments you learn more about the piperine extraction and share how I am to proceed without failure. I have another tincture prepared.

PS: nice glitters

I think my other tincture is ready. I made about 300-400mL this time, but it isn't all the way dark. I might need to add some more pepper sprinkles. I think patience is the biggest key there, and I do everything in small batches. Not looking forward to sucking peppered alcohol vapors through a take-off tube again to get the filter to work though. Setup looks like a bong, I need to get an air pump one of these days.

I wish I knew what went wrong. Just make sure you let it circulate for a couple days to give the little buggers time to clump up. I got clouds with the cedar tincture but they never clumped, and the filtrered stuff didn't look good for anything, except clogging coffee filters. The cloudiness in my water extracts is the same way.

I wasn't going to take a picture of the glitters, but then I thought, EM likes crystally red stuff, he might appreciate this. If the plant salts clarify it a bit then they could end up looking really really nice. I plan on doing all of this again with tumeric, and a plantain extract would be lovely as well. Alchohol extracted resins are always black, nasty, and annoying, but this water extract, even the jelly form, has been awesome. Almost none of the pepper taste comes through, but you can feel the heat on your tongue after a few seconds with the jelly, but the red crystals are sublime. My nervous system feels charged within seconds of taking a finger dip. Those little tingles remind my of building energy in rituals. Might just be a mental thing, but I feel like I'm on to something. See if I can dig up some lead around here. I have a drop of mercury in a pill bottle somewhere around here.

Dragon's Tail
01-09-2018, 01:14 AM
Alright Mr. Mixer, this is for you. Piperine extract trial number 2. This is my second extraction and looks a little light to me. 95%eth solvent, some of the pepper was reused from the first tincture, but I added more to make sure I got a good extract, still not happy with it but we'll see how it goes. After waiting on the tincture forever, I feel like doing something tonight while still trying to purify my water extract Sulphur. I squeezed out the mash and filtered off 150mL total tincture, using a coffee filter and a funnel:

https://i.imgur.com/JIZYenm.jpg

Next step was water bombing. I decided to try something a little sneaky by doing this in a separatory funnel. New idea that came to me a couple days ago while fighting this constant and annoying string of cloudy nonsense that refuses to filter off properly. I put the 150mL of tincture in the funnel, and then put 200mL of H2O (the universal solvent of everything awesome and amazing! haha) into my measuring cup so that I would have some solid numbers for you (despite the tincture that might be on the weak side).

I added about 75mL of water to the tincture, this is the initial result. I'm going to let it sit for a while and see if it settles at all. I'm not worried about clumps because those took days before.

https://i.imgur.com/uFMNWcQ.jpg

You see how it looks darker up there at the top of the creamy part? That's not a camera trick. There's definitely a transition at the top of the creme before the cutoff line at the remaining tincture part (which strangely enough appeared to darken with the water bomb). I may have been using too much water before :/ That's why I'm going to let this settle and see if it separates into a third fraction. The water wasn't added as gently this time either, so it might just be a fake emulsion look that will settle out on its own.

Dragon's Tail
01-09-2018, 02:07 AM
Okay, so that was weird. Nothing seemed to be happening, so I siphoned off the bottom 75-100mL or so into the cylindrical bottle to the left. Added some more water, then poured off ~100 into my flask. 200mL water to 150mL tincture aparently worked perfectly, good guess huh?

Here's the odd part, and sorry for the low resolution. I turned off the bright light. That cylinder got the first cut, but the flask and what is left in the funnel look bright and milky, while the first cut has some darkness in it. Maybe the phlegm settles to the bottom first? So weird, will watch these guys tonight for any signs of separation and see what to do with them in the morning. Probably going to drain off the rest and clean my funnel. Now I'm wondering how much cut would work to clean the phlegm for maximum "good stuff" yield. Might be able to optimize that somehow. Like the first x-mL of water extracts the crap and the rest gets the good stuff? Maybe? Or I might be deceived by the colors. Either way, these guys have some sitting around to do.

https://i.imgur.com/Xqd9Yl1.jpg

And that is how you milk peppercorns, lol.

Aham
01-09-2018, 02:56 AM
I squeezed out the mash and filtered off 150mL total tincture, using a coffee filter and a funnel:

Nice going DT. Pics are worth a 1000 words. The whole water thing is a bit of a novelty for me so am quite interested in how this turns out. Might even take a stab myself.

Have a few questions if you don't mind answering:

- How much pepper did you start with?
- Did you coarse grind the pepper just before use or did you buy it coarse ground?
- How long did you let the mash ferment?
- Any specific temperatures you used to store the mash?

Thanks in advance

Dragon's Tail
01-09-2018, 03:41 AM
Nice going DT. Pics are worth a 1000 words. The whole water thing is a bit of a novelty for me so am quite interested in how this turns out. Might even take a stab myself.

Have a few questions if you don't mind answering:

- How much pepper did you start with?
- Did you coarse grind the pepper just before use or did you buy it coarse ground?
- How long did you let the mash ferment?
- Any specific temperatures you used to store the mash?

Thanks in advance

I think you might be a little confused with the pics. The milk extraction is from the regular old tincture, so no real fermentation...however, I'll try to answer everything the best I can since your questions apply to my parallel experiments.

My primary experiment was 200 mL of store bought ground pepper, because everything is still in testing and it was cheap. The tincture was about 100mL in 95% ethanol. I had a big jar laying around, and I'm still hammering out my process, so using what's available.

Tincture Details--
The alc tincture makes the milk, I usually run tinctures till they are totally dark, but pepper is kind of annoying in that respect, about 2 weeks soak. This milk extracted the piperine, and the tincture has some wonderful qualities, use only a few drops at a time, they go a long way. The piperine crystals are much more mild than you might expect when finished, but still mix them with something.
The tincture "mash" I mentioned was just a cute way of saying the remaining pepper matter leftover from the tincture.

My water extraction details--
The other part of the experiment. 200mL of pepper was added to a flask with just water, bubbled away under reflux. After a few days it makes a kind of sludge that was decanted and closed up (no yeast) and left to sit. I added more water to the remains and kept refluxing until it came off the flask easily. The saved "sludge" was left near my pot while other stuff was going on, range 20-60C depending on what I was doing, and when opened a month later it did have a sharpness to it, like you would expect from a ferment product. Not offensive but not just pepper smell either. I separated the solids by squeezing through a cloth sieve, which came out black/gray, these were incinerated, calcined, leached, and are currently drying on the pot. The liquid fraction was stoppered back up and allowed to continue doing its thing, same spot as before. The sediment in the bottom even reminds me of yeast husks, but the smell isn't alcoholic. It's almost like a vinegar smell, but not quite. This will make my "honey," from which I'll extract the Sulphur, but I'm still working with the test batch to figure that process out. You can dry it all the way on mild heat, then add more distilled water, and filter off some feculance each time, but I'm looking for a better method as I refine the first batch. Meanwhile my good "fermented" honey is sitting there fermenting away until I'm ready for it.

Hope this helps clear things up. I've gotten into a habit of doing a tincture of whatever herb I'm working with otherwise, the piperine crystals were just too good to ignore, which is why I included them in this thread.

The trick with the water, which I haven't figured out yet, is getting the Sulphur purified. After enough solve et coagula you should get something like the little red crysal-looking powder I posted earlier. Even after screwing that up with essential oils, once the oil vaporized off of it, it still has some potency, but you will see that after enough repetition, the dark red mass in the bottom of your drying jar will start to lighten to a golden color on drying. You scrape it out and get the "red earth." I think continuing the process will make it even better, but that first sample (and the current one) didn't undergo any real putrefication, unless you count the sweet smell that comes out on drying them at low heat.

I already know this is going to be a little confusing, but if you have any questions, I'll try to answer the best I can. The better that honey is purifies though, the better the product, and it can be combined with the extracted salts and then evaporated together easily at that point.

Hint: I think the sulphur has to be calcined gently. I'm still hunting for the right temp. Too hot, and you'll burn it.

Dragon's Tail
01-09-2018, 09:36 PM
Back to the water extract. I have a little over 10 grains of the stuff this time, more than last time, but there's still a long way to go. I decided to dry it all the way and powder it. I know it's a fiddling small amount, but I've gotten used to running tests with the tiny stuff. It would take a pretty major "wow" moment for me to start manufacturing more, and even with small amounts, this experiment has a long way to go yet.

This is one powder, but there are actually 2 different materials, or so it seems. One of them runs thick like honey while the other dries out pretty quickly. I'm not sure which I need. The "honey" part appears to dissolve slower in water, so the last time I dissolved them, I did it in two parts. the second is currently on low heat evaporation, this was the first fraction. I'll be comparing for differences. Maybe I can separate them that way, or maybe I'm fooling myself. I think I'm going to try using other solvents on these just to see what happens, and if there is an easy extraction medium. My plan is to use alcohol, and perhaps vinegar and maybe ammonia if that doesn't work. I just have to be real careful with the measurements as there isn't enough material to go around. Another idea is to see if I can bleed it with heat or calcine it, but the gum dried up pretty well, so I don't know if it will melt with more heat or not.

Just a note, when this stuff dries all the way, it's a pain in the butt to get off the glass, so use something sturdy like a shallow mason jar, and be prepared for jumpers while scraping it.

Here it is just after scraping, you can probably see the two different substances mixed together:
https://i.imgur.com/qJpgSTw.jpg

Here is after powdering, the "red earth"
https://i.imgur.com/Hiuiriz.jpg

elixirmixer
01-09-2018, 10:46 PM
I'm loving your work on Black pepper bro. Keep it up, I'll give another shot at piperine soon.

Dragon's Tail
01-09-2018, 11:21 PM
I'm loving your work on Black pepper bro. Keep it up, I'll give another shot at piperine soon.

cool. My "dark" part sorta separated, brighter on the bottom, but I think even that is still darker than the 250mL flask. The dark one is chilling on my desk with a filter paper over it, and the other one is stuffed in a drawer. I haven't applied any heat, just going to let them sit and see if they coagulate a little. Next time I mess with them I will try to filter.

I was reading back through the thread last night and wonder if you had the right stuff but it just didn't make crystals for whatever reason. If it looks "hairy" then you are on the right track for sure.

elixirmixer
01-09-2018, 11:53 PM
I thought I had it, but no crystals, and also, I tasted it expecting it to be like "BOMB" but it was more like "Mehhh" which makes me think it wasn't pipeline. However, I know what I did wrong. Didn't wait long enough for coagulation to occur. I have no idea where the piperine went. Literally no clue.

Dragon's Tail
01-10-2018, 01:22 AM
It might be a little underwhelming depending on your expectations, but it will start a nice burning sensation on your tongue shortly after tasting, and should have a scent.

elixirmixer
01-10-2018, 01:29 AM
Have you found any other tincture-water precipitate extractions that might be useful?

Aham
01-10-2018, 01:52 AM
Damn, that's a bunch of stuff going on :) Yes, will definitely have questions as I try to fully process(in my mind) all the stuff you're doing. Once again, thanks for the detailed post.

Dragon's Tail
01-10-2018, 03:41 AM
Have you found any other tincture-water precipitate extractions that might be useful?

The only one I have that will bomb out is the remaining cedar. I didn't try the mullein yet, but that's a soft plant I'm not even sure if it will do anything. I'm not particularly interested in whatever might be coming from the cedar at the moment, enough to screw with it anyway. No idea what's coming out unless it's that same chemical that's in pine tinctures. As you said, the process can be a little annoying, so scratching my head trying to extract the cloudy may end up fruitless.

Dragon's Tail
01-11-2018, 04:38 AM
Piperine experiment 2. After the ordinary regular old tincture with NOThING special about it (just want to make sure I'm being clear here, pepper tinctured in absolute), solution is waterbombed, and after a couple days of sitting in a sealed bottle in a dark place, I turn the bottle sideways, and...

https://i.imgur.com/kMwO0FE.jpg

Crystals. That seems to be the secret, stuff it in a corner and forget about it. I'm wondering if I should distill off the alc portion, since as I showed before, I bombed the stuff out in two parts, and while I'm not 100% sure, I think the brighter fraction is more of the good stuff and less dross than the last time that I did it. We shall see I guess. If I dry it off instead of filtering and a bunch of crap drops out, then we'll know. The recovered liquor can be used to redissolve and purify them :)

elixirmixer
01-11-2018, 05:11 AM
Ratio?

Dragon's Tail
01-11-2018, 05:26 AM
I put the exact measurements in a post on page 7. I added 75ml of water to 150ml of tincture, iirc. Siphoned off about half of the cloudy in a separatory funnel (actually, around 100ml of the mixture), and proceeded to add another 125ml of water. That's what's in this flask, after the second water bomb. Assuming that the liquid was kept at an even ration (even though the darker portion "floated")... let's see.
75water + 150ml 95% = 225ml 63%ABV - siphoned 100ml
125ml 63% + 125ml Water = 250ml ~30%ABV (measurements after separating in the funnel are approximate)

Roughly 2 parts distilled water to one part pure tincture extract to go all cloudy

EDIT: I tossed the 250ml flask pictured back in a drawer. Will check it again in a week or so and see if the crystals are growing. My very first experiment in alchemy ~12 years ago was with oak leaves, and I found the bottle with the extract years later. A crystal garden had grown in the bottom. I'm a big fan of time and patience.

elixirmixer
01-11-2018, 05:32 AM
Set and forget. Got it. Cheers, I'll let you know.

Dragon's Tail
01-11-2018, 05:38 AM
Go slow, EM. Make sure the crystals are growing, and post pictures for heaven's sake, lol. Are you water bombing tonight?

elixirmixer
01-11-2018, 05:55 AM
Are you water bombing tonight?


Indeed. I still have to do that ether as well so tonight is a lab night.

I can't do pictures right now cause I've been in an eight month battle with Telstra and only have I ternet on my phone and can't click and drag into the input menu

Dragon's Tail
01-11-2018, 06:06 AM
Good luck then. It shouldn't take but 2 or 3 days for the little guys to sprout. Also, it's cold up here in the northern hemisphere, but the flask was sitting at around room temp, and I did nothing to heat it this time. The first pour off was showing some signs, but I didn't want to bother fitting a cork to it. Continuing to let it dry very slowly through a filter paper "lid." There wasn't much in that one at all that I could see by tilting slightly.

Be careful with that ether. Would hate to lose you.

elixirmixer
01-11-2018, 06:25 AM
Yeah I've been putting it off cause I'm pretty scared. Last time I'll be ordering it in those quantities 2.5L bottle.

But on the other hand, it has to be done now or never, they are in two bottles of 1 ltr and 500mls bottles not amber so NoT good. I've only got 1.5 litres left. (Edit)I transfered it from one bottle, into two of smaller volume to try to not die. However, its in a clear bottle, and any exposure to air (pouring) is not good either so, this is why beginners should NEVER play with it. I've been in labwork and chemical practices for a good 7 years, with a 5 year pre study, and you can tell that even I'm struggling.

I'm thinking of grabbing a KG of a few harder to eat herbs aka reshi mushroom, hi WO shu, brahmin. And doing a big extraction, hoping that dropping it I to shitloads of organic matter will stabilize it a bit. And then start doing small evaps. Its hot down here ATM making it very important to get it done now before it decides to dispose of itself.

Dragon's Tail
01-13-2018, 07:13 PM
Some updates on my new batch of piperine. The crystals in the flask in the picture aren't growing, so that's about as much as I can remove by letting them sit at the moment, that was "the good fraction" from my siphoning.

The bad fraction was left to experiment with. I took about half of it and made a room temp solution of saltwater, as much as would dissolve. I added a bunch to the piperine solution and let it sit. After a couple hours, it didn't appear to be doing anything, so I set it off to the side. I checked back today, I believe at least 2 days later, and that solution had clarified, leaving a greenish yellow crystalline solid at the bottom. I believe this is a mix of piperine and pepper tars. I decanded the solution into the remaining "first pour off" as it seems to be effective at precipitating out the cloudy. I just didn't expect the process to take several days.

I'll probably be splitting off some of the solution from the flask in the picture, and try distilling or drying the alcohol fraction off. My suspicion is that the tar will stay with the water while mostly piperine drops to the bottom. Those first crystals are really yellow so I'm going to keep them separate until I'm sure if the distillation method works or not.

Just thought I would add this because the salt solution definitely left a precipitate, but it took days and the jar was not sealed. Might be worth trying in a sealed jar, and I would prepare the saltwater ahead of time to keep NaCl from dropping out with the piperine, even though they can in theory be separated easily because of different solubilities in water.

Dragon's Tail
01-14-2018, 10:50 PM
So my black pepper tincture was produced in two fractions, as mentioned above. I'll refer to these as the dross fraction (the first part that I siphoned off) and the "good" fraction for reference.

The dross fraction was crystallized out using a preparation of salt water, because it was being fussy. This got everything out, and the picture doesn't really do it justice. It's looks green, but it has the right smell, so the filter paper caught a mixture of piperine and tar, but the solution clarified a lot after sitting for 24-48 hours (I did it twice by splitting the dross fraction into 2 separate containers for repeatability, salted one out, then poured the remaining clear fluid into the other. The salt is obviously staying with the fluid)

https://i.imgur.com/lIIn9gL.jpg


The good stuff was in a separate flask, and the little crystals were fixing themselves to the glass. But after a good bit of agitation, most of them came loose. Enough that I didn't feel like scraping out the rest anyway. The filtrate was still super duper cloudy, which means more suspended piperine that is too small to get caught:

https://i.imgur.com/wR6C6iX.jpg


The filter paper looked like this after opening. This solution has been sitting in a dark place for about a week to bring these about, nothing added after the distilled water:

https://i.imgur.com/6qrPOUd.jpg


Here's a picture of the clear salted out dross filtrate on the left, and the "good stuff" filtrate on the right. In the middle is the rest of the dross waiting for filtering.

https://i.imgur.com/WlnvQDy.jpg


I'm still not sure about salting out my good stuff. Next step is distilling the original solvent off the dross fraction, to see what happens. I might split the "good" filtrate into two equal parts and add some NaCl to one, just to see what drops out and how it compares to the dross fraction. I'm suspecting that if you start by adding a little water, let settle, and siphon the lower layer off, you will get a better piperine extract from the rest, that the gum falls out of solution very quickly, but I could be horribly wrong. I suppose we shall find out. The other question is the method of getting out the stuff that doesn't readily crystallize. Salt vs distillation.

Either way. I haven't weighed my "good" crystals (retrieved from a sealed flask after a week of sitting in the dark), but it was a good heaping tablespoon worth. In both cases, removal from the filter paper while it was still wet was super easy. I spread the paper on a plate, and scraped them free with a butter knife, and there was enough that I didn't worry about the fiddly bits that got away. I'm really happy with how this went, the good fraction produced crystals of amazing brightness. They're small, but they have a great color like the ones on wiki.

Dragon's Tail
01-16-2018, 02:34 AM
quintessence from decoction.

I so far have not been successful (I don't think). Things at the final stages keep revealing an off putting odor, but one thing in particular remains sweet.

To catch up, I got the common white salt from the ashes, and the red wine from the rest of the water. The "wine" I've been working with so far was not allowed to rest and ferment of it's own devices, and it can be separated in many ways, but you will notice after refluxing that the fluid becomes thick, almost slimy. This is the portion the next phase of my experiment will focus on.

The solid mass is separated and burned to a calx, making our common alkali salt.

In general though, the reddish liquid, however I extract it, drops a brownish earth. This isn't easily filtered out, but it can be mostly separated through decanting, and then filtering the last bit of solution with only a little of the "earth" remaining. This is dried to a red earth and saved. The remaining fluid is dried to a gum. <not sure separating these two is necessary>

The red earth and/or the gum (I'm not sure which because I mixed them back together, I suspect the gum) contains inside it an oil, even when evaporated to dryness and calcined to over 150C. This oil can extracted via tincture, which then must be put through it's own series of purifications. I think this oil is the key, at least so far it's the only thing that doesn't stink of lysol when mixed.

The white salt and the yellow or red oil are mixed in the proper proportions, and can be further purified through washing with distilled water to the point of purity, leaving a wonderful and precious something upon evaporation.

So ends the theory. The next phase will be repeating this entire process with a red liquor that has putrified to a sharp vinegar and dropped it's red earth. The salts are already mostly prepared, and I start again. I'm worried that I don't have very much left, but perhaps enough to give my speculation above an honest run without killing the necessary ingredients for the final preparation.

A note, the putrefication occurred BEFORE I separated the solids from the refluxed soup. The wine separated too early (what's left of it) has contracted a white hairy mold. Reflux, find the gellateanous goop, and bottle it up tight while it's still hot. That will (I think) allow it to putrefy to sharpness. The bottle was also placed near my heater, so it's been kept warm most of the time, but cooled down when nothing was happening in my heating pot.

I'm pretty sure of the process at this point, so I'm going to go at it again and see if I get enough of the little oil to make something. I won't be doing any of my normal fractioning this time, it's all or nothing. If it proves interesting, then I'll repeat this whole thing again with another plant material, for validation of the process. It's been fun, and if nothing else, I learned a few tricks along the way for purification of products.

Dragon's Tail
01-23-2018, 04:14 AM
Couple of interesting things.

First off, I began by refluxing my putrefied extract of black pepper for a couple days, took it off the heat, and noticed that the "sediment" portion has expanded, either fluffed up or more dropped out? Don't know. My idea is trying to merge everything together over time, so far so good, but it will need more heating.

I've also been working with the piperine leftovers, and noticed a cloud in the distillate. Not cloudy like a hydrosol, but a little bit of cloud in the bottom of the receiver, so something volatized. Some water may have gone over into the product, but time will tell. I've never seen it like that before though, so back to thinking about stuff. The piperine wasn't meant for any kind of alchemical examination, but it's hard not to overlook something new appearing in the flask.

Yes, I'm still at this project for quite a while now, will be taking things slowly, and keep learning in prep for whatever my next crazy adventure will be.

elixirmixer
02-08-2018, 09:55 PM
So I dont know what the fuck is wrong with me but I have failed making piperine. In fact I've been making a lot of epic fails in the lab lately and I think I'm taking a step back to do some personal work before continuing because I followed your instructions to the tee, and same with the volatile salts experiment and Steve kalec and all has gone to hell which makes me think that my energies just are not in sync enough to be performing lab work right now.

elixirmixer
02-08-2018, 10:01 PM
I got the milk, but over time it starts to 'clear' up, however there is no precipitate and adding more water did not "re-milk" the water. I haven't filtered yet but that's because I know its going to fail and I'm trying to work out what's going on here....

Maybe it didn't put it in a dark enough spot?

I'm going to have one more try and then just shoot myself.

Dragon's Tail
02-08-2018, 10:13 PM
I got the milk, but over time it starts to 'clear' up, however there is no precipitate and adding more water did not "re-milk" the water. I haven't filtered yet but that's because I know its going to fail and I'm trying to work out what's going on here....

Maybe it didn't put it in a dark enough spot?

I'm going to have one more try and then just shoot myself.

Wow. I literally just logged in after finding a better filter for my milky solutions and was thinking about posting something in here but refrained... I don't know why this isn't working for you. You have the milky but no precipitate? This was after adding water to pepper tincture??

I know you let it wait because it's been a while since I got an update from you. Mine never made it to a stage of really clearing up, but you should see some kind of precipitate on the walls of the glass. Most of it settles down to the bottom. If it's light in color (might be a little greenish, I've gotten different sorts of precipitate, it's basically a mixture of piperine and any other insoluble alkaloids/chlorophyll or whatever else depending. The same stuff that makes the "black earth" when you boil off a tincture). That should be it. There will be varying degrees of color and crystallization.

Just to be certain, since you seem to be online, you DID turn the flask upside down to check for precipitates? If your solution clarified, then I would expect all of the good stuff fell to the bottom of the flask. I can't imagine it just disappeared. You've actually encouraged me to think about letting these milkies sit longer until everything drops out. Then I won't have to filter them with copy paper (the mullein experiment I'm doing with a similar method right now, produces a resin gum instead of crystals, and doesn't filter easily at all).

Definitely invert the flask to check if anything is stuck to the walls or bottom.. I'm going to ponder this for a bit. I have since seen posts in other forums with a similar process to this for the piper.

EDIT: And do NOT shoot yourself. PM me if you want to talk about anything off topic but need to get it off your chest. I'll be around all afternoon.

elixirmixer
02-09-2018, 05:42 AM
No I would never end my own life. I have too many responsibility and without Kundalini activated I'm not sure I really want to die just now.

There is crap stuck to the bottom but its green.

Let's go back a step. How do YOU make your tincture. You mentioned boiling. I dont boil mine I just pour on about 80% alcohol or something close to that and then let sit in a warm place for a while (sometimes a long while like my first attempt) I dont boil it.

Is there any way to check if this green stuff has puperine? There does appear to be some "crystally" looking shit in the green stuff but I'm not sure if that's it or not really. If I had a way to check..
.
..

Dragon's Tail
02-09-2018, 06:08 AM
No I would never end my own life. I have too many responsibility and without Kundalini activated I'm not sure I really want to die just now.

There is crap stuck to the bottom but its green.

Let's go back a step. How do YOU make your tincture. You mentioned boiling. I dont boil mine I just pour on about 80% alcohol or something close to that and then let sit in a warm place for a while (sometimes a long while like my first attempt) I dont boil it.

Is there any way to check if this green stuff has puperine? There does appear to be some "crystally" looking shit in the green stuff but I'm not sure if that's it or not really. If I had a way to check..
.
..

It's in there. You aren't using white pepper by chance are you? It has a lower concentration of piperine, IIRC

so, for the piper extract, yes, regular tincture with 95% (190pr), left to sit for as long as it takes. Filtered off the rest of the pepper, then waterbombed the extract. The picture on the top of page 9 is probably what you will see when you filter it. Sounds like you got a lot of darkness in yours similar to what I got when I tried distilling off the liquor, that's why I'm suspecting your pepper source. But it's fine. A tiny amount of the stuff is wonderful. My first extract attempt only got about a grain. How much tincture did you start with?

Anyways, it's dark because there are other alkaloids and stuff that must have dropped out. Since I've had some success purifying my product, I'll give you that process. Those dark alkaloids from my pepper are actually more soluble in alcohol than the piper, so after you filter the mass off, you have some options for purification and recrystallizing. I'd let it dry out first and see what you get. Remember my first one was more of an orange color? That's that darkness.
I think the water balance makes a difference, but I don't have a fool-proof method, thus the complicated fractioning of my last test...

anyway, purification. Take your clump that you end up with, maybe weigh it first, and pop it in a new flask with a little bit of clean alcohol, swirl and let it sit. See what seems to be dissolving, and depending on how dark it is, I would say dissolve about half, and then filter again. If you have darks in the filter, then the good stuff went into the liquid, and you can evaporate it off to recrystallize, but I think you'll find that the darkness "washes" off of the piperine. It did for me anyway. the liquor was yellow-green. The more times you do this step, the more the piper will brighten. I've since found out that you can get it almost to a pure white with just a slight yellow hue.

But, the piperine is definitely in your precipitate. The "crystally" looking shit sounds like a perfect description of it. My first try looked like a clump of brine shrimp that we used to feed to our pet fish after it dried.

I've been working so many tinctures this way now, and I've caught everything from green-black soup to pretty crystals in my filter paper depending on the plant matter in the extract. ALL of it is amazing medicine, even if it's only a lump of chlorophyll. I haven't done too much refinement with the others, but piperine is so damned neat that I had to, and the process has challenged all of my presumptions about the spagyric process.

The pepper I used was also a little aged, so maybe some of the other alkaloids in mine disintegrated with time or something, I don't know, but it was regular ground black pepper. I'm sure you have it, but not sure of the percentage.

Curious, how long did your mixture take to clarify all the way?

EDIT: the smell should tell you if you're on the right track after you filter it ;)

elixirmixer
02-09-2018, 06:26 AM
Its so hot and the kids are so loud... But if I can try and hear my.own thoughts I think they are saying:

Organic crushed black pepper - check
Alcohol, let sit then water bomb - check
Clarification - doesn't go to clear, goes to a murky orange/yellow (the color of piper, which is what is wigging me out and why I ignored the green shit.
Crystals shit - may not be crystals. Trying to find the power source to my microscope but too hot and bothered right now. I've had one of those days where you spend all day looking through your shed filled to the brim with shit just to find stuff you thought you knew exactly where it was.

I have what looks a bit more promising in a chamomile tincture. Seems something that looks quite crystalline has precipitated over time to the bottom of an already filtered tincture. I want to see if I'll have more luck with that and then water bomb the rest and see how I go.

I could have very well fucked it just by not putting it in the dark.

I'll scrap up my two batches of green shit and try a wash and then I'll get back to you but that might take me some time. I need to clean the lab again and fi ish off this essay for Awani(&Co.)

What does the piperine taste like? You said smell.. What kind of smell?? Your always commenting about smells, as if your a bloodhound or something so I'm not sure I'll be able to compare but its still worth knowing just in case.

Dragon's Tail
02-09-2018, 06:42 AM
Its so hot and the kids are so loud... But if I can try and hear my.own thoughts I think they are saying:

Organic crushed black pepper - check
Alcohol, let sit then water bomb - check
Clarification - doesn't go to clear, goes to a murky orange/yellow (the color of piper, which is what is wigging me out and why I ignored the green shit.
Crystals shit - may not be crystals. Trying to find the power source to my microscope but too hot and bothered right now. I've had one of those days where you spend all day looking through your shed filled to the brim with shit just to find stuff you thought you knew exactly where it was.

I have what looks a bit more promising in a chamomile tincture. Seems something that looks quite crystalline has precipitated over time to the bottom of an already filtered tincture. I want to see if I'll have more luck with that and then water bomb the rest and see how I go.

I could have very well fucked it just by not putting it in the dark.

I'll scrap up my two batches of green shit and try a wash and then I'll get back to you but that might take me some time. I need to clean the lab again and fi ish off this essay for Awani(&Co.)

What does the piperine taste like? You said smell.. What kind of smell?? Your always commenting about smells, as if your a bloodhound or something so I'm not sure I'll be able to compare but its still worth knowing just in case.

What does it smell like? It smells peppery even when dry but it won't make you sneeze.
What does it taste like? Very hot like capsacin, but hotter as the color lightens after purification.
The crystals are also very tiny, my pics are all taken up-close.
Also, the picture I mentioned at the top of the page, the camera messed up, I remember that batch being incredibly green and dark.
Dark storage? I'm careful about this, but darkness won't hurt piperine nearly as much as heat, I've discovered. It's pretty stable at room temp.

When I did my purification I did it a tiny amount at a time and it took for ever, but then I tried to tincture the finally pure product. It doesn't dissolve very quickly after you make it. I think the crystals, tiny and fragile as they are, really like staying crystals and they don't want to redissolve unless you crush them into a powder.

Sorry that you're having a bad day, man. The chamomile sounds interesting, I might do a google hunt and see if I can guess the compound that might be crystallizing out. My next try will probably be tumeric once I finish my current 3 experiments.

elixirmixer
02-09-2018, 07:23 AM
Thanks.

Tumeric would suit very well with your piperine. To me the entire purpose of piperine is to enhance the effects of tumeric.

I'm going to go filter that chamo now and see how we go.

Dragon's Tail
02-09-2018, 03:03 PM
Thanks.

Tumeric would suit very well with your piperine. To me the entire purpose of piperine is to enhance the effects of tumeric.

I'm going to go filter that chamo now and see how we go.

Cool. Depending on how dark it is, you might only end up with a little bit after cleaning it. If you have enough to grow crystals, the chem people use acetone as a solvent for that. I had some results with alcohol but nothing like the flask picture on wiki.