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Microscale MHRB Dry Tek Experiment


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#1 Phineas_Carmichael

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Posted 15 March 2011 - 06:00 PM

What follows is a report from my buddy Freddy concerning a silly little experiment he did. He has performed an STB on a small amount of MHRB, treating it like the beginning of a "dry" cactus extraction. He is aware that there are better ways to do this, he just wanted to show that there are more than 3 ways to skin a cat.

18.3g of MHRB:
DSCN2435.JPG

Was mixed with 20g Pickling Lime (Calcium Hydroxide)
and 45mL Reverse-osmosis filtered water:
DSCN2440.JPG

This was deemed to be too much water and the beaker was left to dry out overnight:
DSCN2461.JPG

A splash of toluene was added:
DSCN2462.JPG
And mixed around for 5-15 minutes.
This was repeated 3 times.

The toluene was evaporated:
DSCN2535.JPG

DSCN2541.JPG

DSCN2544.JPG

And the product scraped and quantified:
DSCN2559.JPG

This makes the yield 0.54% on bark that Freddy knows to contain 2% alkaloids. Longer soak times with the toluene would certainly improve the yield a bit. This bit of silliness was brought to you by :smokin:

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#2 TurkeyRanch

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Posted 15 March 2011 - 06:15 PM

Epic sir. :bow:

Truly an asset to the community Phineas.
Are you going to pull again to get the remaining 1.5 %?

:pirate:

#3 Defiance

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Posted 15 March 2011 - 06:22 PM

Very nice!

#4 Mr Kush

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Posted 15 March 2011 - 06:26 PM

Awsome! Thanks 4 sharing!!:rasta:

Is their a particular reason why freddy used tuolene over naptha for this experiment?

#5 Phineas_Carmichael

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Posted 15 March 2011 - 06:30 PM

Thanks guys. Freddy's kind of excited about this, in an abstract way, because replacing the toluene with d-limonene would make this a "food safe" dmt extraction. :amazed:

As far as the other 1.5% is concerned, this is a source of bad blood between Freddy and myself. He got drunk on the sloop one night and rushed through this extraction in an intoxicated fervor. In his drunken state he forgot a primary rule and washed the glassware before the extraction was finished, discarding the botanical mush. :spank:

He says "At least its proof of concept, dude!"
And I say, "Yeah, but think how much stronger that proof would have been if you hadn't been a drunken idiot!"Posted Image


Long story short, this one will take some verification from other Topiates. If anybody has piles of MHRB lying around, consider sacrificing a few grams for science...

*EDIT* Hi Mr. Kush! Freddy used toluene because it happened to be the jug he grabbed at random through the booze-haze :drk:

#6 pharmer

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Posted 15 March 2011 - 06:56 PM

sometimes faster is better than thorough. and if one keeps the paste he can keep pulling from it at his convenience.

this looks like a winner.

#7 trappinfoxes

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Posted 15 March 2011 - 07:04 PM

lol, dude, you're fuggin crazy, that's awesome.

#8 Dr.Hallucination

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Posted 15 March 2011 - 07:12 PM

Very cool PC.:eusa_clap

#9 StheNC

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Posted 15 March 2011 - 09:45 PM

Long story short, this one will take some verification from other Topiates. If anybody has piles of MHRB lying around, consider sacrificing a few grams for science...


I'm a topiate. And I have piles of MHRB lying around. Plenty of naphtha too. I would be more than happy to sacrifice 50 or 100 grams for science. Now I just need to find some pickling lime...

Do you think lye would work in this case? I have a pile of that too.
I should use the calcium hydroxide first though in order to verify these results.

#10 golfyob

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Posted 16 March 2011 - 01:41 AM

:bow::headbang::loveeyes:
You ARE a scientist indeed!!! I am also anxious to start micropulls anyway!
my questions will be almost identical ie; i have only naptha to grab in my drunkin haze.? also lye is in da house.? pickling lime on the way...if needed???
are the proceedings ideal?
love your "crazy" idea's! :headbang::weedpoke:

#11 ktbase763

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Posted 16 March 2011 - 04:36 AM

Phineas, you are the extraction man! I would like to try this microtek; it seems like baking a batch of cookies compared to making a wedding cake. I do love the a/b tek, tho...and this is surely stb...
Love your work, mate!


#12 Phineas_Carmichael

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Posted 16 March 2011 - 08:37 AM

I'm a topiate. And I have piles of MHRB lying around. Plenty of naphtha too. I would be more than happy to sacrifice 50 or 100 grams for science. Now I just need to find some pickling lime...

Do you think lye would work in this case? I have a pile of that too.
I should use the calcium hydroxide first though in order to verify these results.

Awesome, hooray for independent verification! :headbang:

Personally, I wouldn't use lye for this protocol. If you do things exactly as Freddy did, just replacing Ca(OH)2 with NaOH, you will end up adding water to dry lye. We both know this is a Bad Thing. Now, if one were to create a strong lye solution and use that to make the MHRB pasteā€¦ I still wouldn't use lye if I had my druthers. Be safe and careful StheNC!

Pickling Lime around these parts lives at the grocery stores near the canning jars.

:bow::headbang::loveeyes:
You ARE a scientist indeed!!! I am also anxious to start micropulls anyway!
my questions will be almost identical ie; i have only naptha to grab in my drunkin haze.? also lye is in da house.? pickling lime on the way...if needed???
are the proceedings ideal?
love your "crazy" idea's! :headbang::weedpoke:

Are the proceedings ideal? Certainly not. 0.54% yield from bark that has upwards of 2% alkaloids means Freddy only got about 25% of what he could have from this 18.3g of bark.

Naphtha would be perfectly adequate for this experiment, and it won't take 3 days to dry enough for scraping like the toluene did. It might even be possible to freeze-precipitate if naphtha is used. Again though, I wouldn't use lye for this unless I was absolutely sure I was using in a way that won't make it volcano.

#13 StheNC

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Posted 16 March 2011 - 09:07 AM

I thought about the lye, and making a solution first before making the paste. MHRB/Lye volcanos are very bad news.
Maybe I'll do two 25 or 50 gram batches side by side, one with the lye, one with the lime.

Limonene for a "food safe" extraction would be interesting too. I've never used it. Does it leave your alkaloids smelling like oranges? When evaporated, would the consistency of the finished product be like the evaporative product of other solvents or do you wind up with a sticky, orange scented, pile of goo that needs cleaning?

I have never seen toulene around my way, but xylene is easy enough to come by. Is this anything like toulene? I would like to replicate your experiment as closely as possible, as far as the chemicals go. I plan to adjust the lengths of time as well as the number of times things are done.

#14 Phineas_Carmichael

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Posted 16 March 2011 - 09:27 AM

I thought about the lye, and making a solution first before making the paste. MHRB/Lye volcanos are very bad news.
Maybe I'll do two 25 or 50 gram batches side by side, one with the lye, one with the lime.

Very bad news indeed. I'd be curious to see if lye works for dry-teks, if nothing else, using a lye solution will make it easy to turn the extraction into a standard STB if something goes wrong...

Limonene for a "food safe" extraction would be interesting too. I've never used it. Does it leave your alkaloids smelling like oranges? When evaporated, would the consistency of the finished product be like the evaporative product of other solvents or do you wind up with a sticky, orange scented, pile of goo that needs cleaning?

I've never used limonene and neither has Freddy. I don't know if limonene evaporates completely or leaves a residue of orange oils, this is yet another aspect of this drunken brainstorm that requires outside experimentation. :shy:

If limonene does not evaporate cleanly, it might be necessary to salt the alkaloids out of the limonene with vinegar. This would be a food safe tek, but the final product would be DMT Acetate, a decidedly useless form for smoking and empirical quantification. This acetate could then be based with NaOH and recovered with Naphtha (probably for a very clean product) but the extraction would no longer be "food safe."

I have never seen toulene around my way, but xylene is easy enough to come by. Is this anything like toulene? I would like to replicate your experiment as closely as possible, as far as the chemicals go. I plan to adjust the lengths of time as well as the number of times things are done.

Toluene and Xylene are basically the same thing as far as DMT extractions go; DMT and other Mimosa alkaloids are equally soluble in toluene and xylene. The main difference is the boiling point (xylene's is 20-30 degrees higher) and the smell. Xylene is the stinkiest solvent I've ever smelled. I read somewhere a while ago that toluene vapors (while flammable) are non-toxic. (*EDIT* This is not true, disregard. Toluene is toxic)

I'm excited to see your experiments StheNC. FOR SCIENCE! Adjust whatever you feel is necessary; like I said, I'm pretty pissed at Freddy for boozing it up during a theoretical extraction. I can't be too upset though, without a little ethanol, he never would have tried such a silly protocol. Good luck!

Edited by Phineas_Carmichael, 16 March 2011 - 09:34 AM.
correction


#15 Norman

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Posted 16 March 2011 - 10:06 AM

Limonene needs to be salted.

I'd be curious to see a side by side using toluene and acetone.
Acetone evaps a lot quicker and yields like mad, but it pulls so much, a lot of cleanup is needed.

#16 Defiance

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Posted 24 March 2011 - 08:20 PM

Okay, I've got my dry extraction freezing out As We Speak.

I prepared it with 50g powdered MHRB, 50g CaOH, and 100g water. I let it sit overnight until dry and pestled it into a fine powder.

I tried pulling first with gravity filtration. I got 75ml of naptha almost boiling hot, loaded the MHRB powder in the filter paper and dumped it through. It took about 10 minutes to drain through and the powder retained 25ml.

I dumped it through 5 more times, heating in between the pulls, and ended up with ~50ml of slightly yellow solvent that didn't freeze out so much as a single crystal. Oh well.

I tried again with another 50ml (plus whatever is still retained in powder) except this time I mixed it into a paste and let it sit for a couple days, covered. I pulled out the Big Guns and vac filtered this time through and got just under 40ml back. The solvent is much cloudier this time, I'm sure it'll give up crystals.

I won't have any yields until tomorrow, but this was a really simple extraction. My only complaint so far is at how much solvent the powder retains. I'm thinking about saturating with basic water and running it through the vac filter again to see if I can get any more of the naptha Unstuck.

#17 Phineas_Carmichael

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Posted 24 March 2011 - 08:42 PM

:headbang: :headbang:

Thanks so much for testing, Defiance! :hugs:

By letting the powder dry completely, you've done things a little differently than Freddy did. It wasn't clear in my write-up of his process (my apologies :eusa_pray) but the mixture in the beaker was still a paste and not a powder when he added the toluene. "Dry out overnight" meant lose some, but not all, of its moisture. This failure to communicate accounts for the amount of solvent "eaten up" by the powder in your first attempt at least… Chalk that negative result up to my failure to communicate Freddy's Drunken Process properly. :shy:

The second attempt you described sounds much more promising. The long solvent+paste soak time replicates the recommended "dry-tek" procedure for cactus extraction. Can't wait to see the results!

Again, many thanks for testing this drunken silliness. "You must spread some Reputation around" and all that jazz...

*EDIT* Turning the solvent-saturated paste into a standard STB would be a great way to test the process. If most of the product comes out in the aqueous STB we'll know this is just a bit of :weedpoke:

#18 StheNC

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Posted 24 March 2011 - 08:52 PM

Yeah, I'm thinking if the bark was still moist with water it would give up just about all of the NP solvent. I've been meaning to try my own replication, but I've had my hands full with so many other things lately.

#19 Defiance

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Posted 24 March 2011 - 08:53 PM

Good call, I'll make sure and extract the paste and see what turns up. No problem, this is worth testing for sure.

Yeah, I'm thinking if the bark was still moist with water it would give up just about all of the NP solvent. I've been meaning to try my own replication, but I've had my hands full with so many other things lately.


:thumbup: I'll try to re-wet it and give that a shot too, see if I can squeeze out any more solvent before turning it to a more traditional extraction.

#20 Defiance

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Posted 26 March 2011 - 12:11 AM

Got a couple things. First of all, the freeze is done and I definitely crashed out some DMT. Second, re-wetting the paste with water, letting it sit, and vac filtering got me most of my solvent back. I've reduced the volume of solvent down to 20ml from ~70 and I'm freezing out everything I pulled one last time, all together. Pics and final yield tomorrow, then I'll run the extracted paste through an A/B to see what I can squeeze out, if anything.




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