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Where did I go wrong in my extraction? Options
 
EntitySeeker
#1 Posted : 8/31/2017 2:28:51 PM

:)


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EntitySeeker wrote:
***EDIT / SOLUTION***
So I’ve finally cracked the problem! In this case, the success in extraction 100% comes down to the material used.... the following data is from wild, typical variant Acacia Acuminata, harvested in Spring during late afternoon hours.

___________
Material --- Alkaloids Extracted (via 5x Shellite/Naphtha pulls)
________________
Fresh Twigs: 0%
Dry Twigs: 0%
Fresh Bark: 0.333%
Dry Bark: 0.%
Freshly Picked Phyllodes (leaves): 0.015%
Dead Ground Phyllodes (leaves): untested
__________

....If it is possible to harvest fresh bark sustainably, then that is the golden option. There are plenty of fallen branches and trees if a little hunting is done in the native region.




My first 100g extraction failed as I rushed the pulling stage and ended up with a nasty amount of caustic soup in the product, lesson learned. This time I was much more patient.. after performing the same extraction with 250g I was shocked that I couldn't find a milligram of spice! I ran earthwalkers 100g ATB tek (link: https://www.dmt-nexus.me...aspx?g=posts&t=58064). As I have a 5L glass container handy and access to literally hundreds of wild acuminata trees I adapted the tek to suit 250g of plant matter. Meaning I multiplied all amounts by 2.5, still soaking for a good 2 hours in acid and another 2 hours as bassified soup. I'm trying to pinpoint where I messed up and have narrowed it down to 2 potential causes...

1) Using powdered twigs and not bark. I don't want to damage any trees and heard on here that twigs have some of the highest alk content by weight. I only harvested bundles of dead twigs that had already fallen or broken away from the tree. Am I incorrect regarding the alk content of twigs? Or was I meant to be picking fresh twigs only?

2) Skipped the recrystallizing stage. After 5 pulls I fan dried 50% of the naps and put the remainder straight into the freezer. The naps had a milky whiteness to it, which had me feeling very optimistic. 36 hours later I poured all the naps off, tipped the tray upside down, and fan dried for half an hour. Nothing. No crystals, powder or even oily sludge.. So now Im thinking, is the recrystallising step mandatory if tipping off the naps? Did I just pour ~4-5g of spice down the drain?

Besides those few adjustments, I followed the tek to the letter. Apologies if these are obvious questions, I've been reading up on here as much as I can but could really use some help! Cheers Thumbs up
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
melotikaci
#2 Posted : 8/31/2017 3:26:29 PM

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EntitySeeker wrote:
My first 100g extraction failed as I rushed the pulling stage and ended up with a nasty amount of caustic soup in the product, lesson learned. This time I was much more patient.. after performing the same extraction with 250g I was shocked that I couldn't find a milligram of spice!

Not trying to be mean or something but you didn't really learn anything if you tried extracting from 2.5 times more material instead 20-50g after you failed first time Very happy

Ok, now regarding the second question:
1. I'm unable to open the tek link but shouldn't the recrystallizing step be after getting spice out of the freezer? what where you going to re-x if you didn't have any spice in the first place? Did you mean defat?

2. if nothing precipitated(no dmt crystals visible on the bottom of the dish) after 36 hours, why did you decide to remove all the solvent and dry the empty dish?
 
Foetal1tyx
#3 Posted : 8/31/2017 3:45:04 PM
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Having only done 3 extractions, the first going horribly wrong with nothing to show for it but the other two giving me maximum weight ( although using foolproof MHRB with an STB tek) one thing that I learned was if the tek says two hours, let it soak for a day or so. You have nothing to lose.

I too cannot access that TEK but Im assuming you separated the acidic solution from the raw material after two hours before basifying the solution.

Without being an expert, I would just think that its possible you didnt extract much in the initial phase.

My condolences tho. The sheer horror after all that workShocked
 
Loveall
#4 Posted : 8/31/2017 7:28:22 PM

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Did the twigs come with the phyllodes? I'm growing AA also (largest only up to my knee now) and I understand most of the content is in the green areas. Do you know which variety you have?
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
EntitySeeker
#5 Posted : 9/1/2017 6:19:35 AM

:)


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Thanks for the feedback everyone
Apologies the broken tek link, this one should work: https://www.dmt-nexus.me...aspx?g=posts&t=58064
Otherwise this one: https://archive.is/sQ4jN

melotikaci wrote:
Not trying to be mean or something but you didn't really learn anything if you tried extracting from 2.5 times more material instead 20-50g after you failed first time Very happy


Yes I probably should have started smaller Big grin I was very confident and had lots of free plant matter available so thought what's to lose? Well clearly I've lost/wasted a lot of chemicals... ah well, next time I'll run with 50g and see how things go.

melotikaci wrote:
1. I'm unable to open the tek link but shouldn't the recrystallizing step be after getting spice out of the freezer? what where you going to re-x if you didn't have any spice in the first place? Did you mean defat?


Sorry I used the wrong terminology, yes I was referring to clean up stage / defat.

melotikaci wrote:
2. if nothing precipitated(no dmt crystals visible on the bottom of the dish) after 36 hours, why did you decide to remove all the solvent and dry the empty dish?


Was just following the tek.. thought crystals may have been too small to see, translucent or trapped in oily film on the bottom.

Foetal1tyx wrote:
let it soak for a day or so. You have nothing to lose.


If there's nothing to lose, I will definitely take your advice and soak for a day. I feel it would be a lot less stressful running this sort of procedure slowly over a couple of days rather than cramming it into a single afternoon/evening.

Foetal1tyx wrote:
I too cannot access that TEK but Im assuming you separated the acidic solution from the raw material after two hours before basifying the solution.


No I didn't.. The tek didn't call for this though? Neither does cybs ATB tek?

Loveall wrote:
Did the twigs come with the phyllodes? I'm growing AA also (largest only up to my knee now) and I understand most of the content is in the green areas. Do you know which variety you have?


I'm not 100% on the variety I'm using but fairly sure it is the typical variant. I wasn't aware about that rule of thumb for green areas. From what I've researched, bark and small twigs have the highest concentration by dry weight (1.5-2%). Phyllodes having anywhere between 0.2 and 1.5% depending on plant location, genetics, and season (with the highest alkaloid concentration anecdotally reported in summer and the lowest being winter). The twigs I picked weren't necessarily near any phyllodes, they were attached to larger sticks / branches that had fallen to the ground or had broken off the tree and accumulated in bundles stuck in the branches. Those dead twigs could have been sitting there for years which is why I'm worried they might be non-viable.
 
EntitySeeker
#6 Posted : 9/8/2017 2:04:21 PM

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So a few days ago I did two 50gram extractions side by side, taking note of some of the advice on here. In one of the 1L bottles there were powdered dry twigs collected from one tree, and in the other, I used powdered fresh (green) twigs collected from a recently dead tree.

Basically, I ran the tek as it is with these modifications:

-Cold acid soak overnight
-Warm water bath of acid soup extended to 2 hours
-Warm water bath of caustic soup extended to 4 hours, re-warming at the 2 hour mark
-Let the caustic soup cool COMPLETELY outside of the warm water bath for a full hour to room temperature (now sitting for a total of 5 hours), and heating up Naps very hot for optimum pulling power
-Sat the pulls to precipitate in the freezer for a good 36+ hours.

Still absolutely nothing, aside from a minute quantity of what seems to be oil/plant fats from the green twigs extraction. I'm thinking the only possible reason must be bad bark/twigs and an incorrect plant ID. I guess I'll take some photos of the trees and get an ID confirmation to rule out whether or not this is the problem.
 
downwardsfromzero
#7 Posted : 9/8/2017 4:07:39 PM

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I can't believe you just dumped all the naphtha down the sink:
Quote:
So now Im thinking, is the recrystallising step mandatory if tipping off the naps? Did I just pour ~4-5g of spice down the drain?

Rule 0: never throw anything away until you're absolutely sure it's ok.

Also, that's really bad waste disposal practice. Never, ever, tip naphtha down the drain.

You can re-use naphtha, you know. Even after a successful freeze precipitation the naphtha will still contain a small amount of DMT which is, ultimately, recoverable.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Ulim
#8 Posted : 9/8/2017 4:23:47 PM

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Sad As downwardsfromzero said.
You dont want to harm the acuminatas but then you pour tons of naptha down the drain Neutral
If you need to get rid of naptha keep it in the bottle you got it in and then use it to start a grill or power a lamp. Or simply burn it.

You might want to use "fresh" twigs.
The DMT doesnt degrade quickly in material thats fresh harvested and dried but i think twigs and bark that laid outside in sun and weather will nearly loose all the DMT quickly.
Go for phyllodes and follow the tek with extended soaks. Twigs are afaik not that high in alkaloids. They are concentrated in bark rootbark and phyllodes.

If you pull some base soup during the pulling stage simply pour all back into the big container and let it seperate then start again with clean dish and baster/pipette.
 
Loveall
#9 Posted : 9/8/2017 6:05:05 PM

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Incase it helps with identification, here are the pictures of my AA narrow leaf variety. Some green tips are turning Brown and curling but the plant looks healthy overall.
Loveall attached the following image(s):
IMG_20170908_123738780_HDR.jpg (3,702kb) downloaded 113 time(s).
IMG_20170908_123643154.jpg (5,524kb) downloaded 113 time(s).
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Loveall
#10 Posted : 9/8/2017 6:20:35 PM

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EntitySeeker wrote:

Still absolutely nothing, aside from a minute quantity of what seems to be oil/plant fats from the green twigs extraction. I'm thinking the only possible reason must be bad bark/twigs and an incorrect plant ID. I guess I'll take some photos of the trees and get an ID confirmation to rule out whether or not this is the problem.


The oil residue could be promising. Sounds like what you should get when working with Acacia and not washing the acid soup with solvent and then doing hot naphtha pulls (if I understand your procedure right). Does the oily residue have a "spice" smell (like what a sexy alien's used sneakers would smell like: tones of pungent plastic yet oddly pleasant)? How much does it weigh (~1g)? Any pictures? You could try to clean it up further.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
EntitySeeker
#11 Posted : 9/10/2017 4:53:20 AM

:)


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Thanks everyone. Next extraction I will experiment with phyllodes in one container and bark in the other, with extended soaks.

downwardsfromzero wrote:
Also, that's really bad waste disposal practice. Never, ever, tip naphtha down the drain.

You can re-use naphtha, you know. Even after a successful freeze precipitation the naphtha will still contain a small amount of DMT which is, ultimately, recoverable.


Noted, I'll re-use my Naps from here onward. I would have thought re-using each time would result in a build up of impurities?

Ulim wrote:
You might want to use "fresh" twigs.
The DMT doesnt degrade quickly in material thats fresh harvested and dried but i think twigs and bark that laid outside in sun and weather will nearly loose all the DMT quickly.
Go for phyllodes and follow the tek with extended soaks. Twigs are afaik not that high in alkaloids. They are concentrated in bark rootbark and phyllodes.


Well my extraction on 50 grams of fresh twigs yielded nothing so I'm definitely thinking the twigs should be avoided now.

Loveall wrote:

The oil residue could be promising. Sounds like what you should get when working with Acacia and not washing the acid soup with solvent and then doing hot naphtha pulls (if I understand your procedure right). Does the oily residue have a "spice" smell (like what a sexy alien's used sneakers would smell like: tones of pungent plastic yet oddly pleasant)? How much does it weigh (~1g)? Any pictures? You could try to clean it up further.


Yeah I take it as a good sign that there is some sort of residue, as the defat stage was skipped. There's very very little - not worth cleaning up (I'm guessing less than 100 milligrams). Honestly it just smells like the Naphtha.
 
Tryptallmine
#12 Posted : 9/11/2017 2:51:29 AM

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melotikaci wrote:
EntitySeeker wrote:
My first 100g extraction failed as I rushed the pulling stage and ended up with a nasty amount of caustic soup in the product, lesson learned. This time I was much more patient.. after performing the same extraction with 250g I was shocked that I couldn't find a milligram of spice!

Not trying to be mean or something but you didn't really learn anything if you tried extracting from 2.5 times more material instead 20-50g after you failed first time Very happy

Ok, now regarding the second question:
1. I'm unable to open the tek link but shouldn't the recrystallizing step be after getting spice out of the freezer? what where you going to re-x if you didn't have any spice in the first place? Did you mean defat?

2. if nothing precipitated(no dmt crystals visible on the bottom of the dish) after 36 hours, why did you decide to remove all the solvent and dry the empty dish?


In fairness - 25-50g of twigs and phyllods is going to net you pretty much close to nothing. Anytime I've extracted from phyllods or twigs I've had to use 250-500g with an enthanol presoak. These parts of plants while sustainable, simply don't have the same percentages of alkaloids as root bark. 100g of quality root bark might yield you 1.5%, you'd be looking at perhaps 0.4-0.6% at best from twigs and phyllodes.
 
EntitySeeker
#13 Posted : 10/7/2017 3:18:41 PM

:)


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(One sentence summary at the end)

So I’ve finally cracked the problem! In this case, the success in extraction 100% comes down to the material used.

An extraction on 50 grams of freshly picked phyllodes with extended soaks - yielded a measly 30 milligrams of oily white film (approx 0.015%). This was scraped into a waxy brown goo (it’s possible that small particles from the caustic soup contributed to the brown colour). Unless the tekker wants to harvest kilos of phyllodes at a time, I think they are an ineffective method for spice production. If phyllodes are richer in alkaloids during the summer (as is reported anecdotally), then maybe they’d be worthwhile.

PIC OF UNSCRAPED FILM: https://i.imgur.com/fsLT1O8g.jpg
(also attached below)

A week or so after the unsuccessful phyllode extraction I stumbled across a huge Acuminata that had one of its larger branches recently chainsawed off. Probably done by a ranger / government worker as the branch was growing close to the road and might have represented a hazard to traffic. The huge branch was lying where it fell to the side of the road, so I ripped off a few big chunks of bark to test. This was not the same sort of bark as I was previously experimenting with (dry, dead bark that was practically peeling from the tree). This was fresh, alive bark - literally smelling like Raspberry Jam. I peeled bark off all the way down to the white core of the branch. The powdered bark was soaked in a cold acidic solution (pH3) for 3 days, introduced to a warm water bath for an hour or two before salting + bassifying, then the bassic soup (pH 13) sat cold for a further 3-4 days. From 150 grams of bark around 450 milligrams of small yellow crystals were pulled. A bioassay proved they are indeed psychoactive!

PIC OF UNSCRAPED CRYSTALS: https://i.imgur.com/ap1JuKQ.jpg
(also attached below)

So to summarise... the following data is from wild, typical variant Acacia Acuminata, harvested in Spring during late afternoon hours.

___________
Material --- Alkaloids Extracted (via 5x Shellite/Naphtha pulls)
________________
Fresh Twigs: 0%
Dry Twigs: 0%
Fresh Bark: 0.333%
Dry Bark: 0.%
Freshly Picked Phyllodes (leaves): 0.015%
Dead Ground Phyllodes (leaves): untested
__________

In light of my experience, I believe that the statement I’ve seen on this forum regarding Acuminata twigs having the highest percentage of alkaloids by weight is merely an assumption - and inaccurate. However more tests / replication are required to say anything definitively. Phyllodes are barely worth the effort and large quantities are required. If it is possible to harvest fresh bark sustainably, then that is the golden option. There are plenty of fallen branches and trees if a little hunting is done in the native region.

I’ll edit the following info into the first post so that other may learn Smile

TL;DR
Use fresh bark - other sources (phyllodes, dead bark) not practical for extraction.
 
 
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