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official extraction help thread Options
 
downwardsfromzero
#3341 Posted : 10/15/2021 11:59:14 PM

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Nordic traveller wrote:
Hi everyone! I recently did my first small MHRB extraction using Noman's tek and was pretty happy with the result. From what I've gathered from reading the Nexus you can increase yield and/or make the extraction faster by salting the base solution with for instance NaCl (without iodine). I'm planning to try that next time. I have a couple of questions.

-Is more NaCl better? (If not, what is the optimal amount?)
-Is it ok if the solution saturates with NaCl and some salt crystals are left on the bottom of the bottle during pulls?
-Are there other salts or combinations of salts that are known to be better than NaCl?
-Are there any known disadvantages to salting the base solution?

You've been answering several questions here so it seems fair that your own questions should get answered too!

A lot of what you're asking about is answered here: Minimum Polymer
so it seems that keeping the salt concentration down might be desirable if you'd rather get white fluffy crystals. Hence, saturation is unnecessary, and I would suggest that salt crystal formation has the potential to be unhelpful in the extraction.

Sodium chloride is useful on account of its ubiquitous availability and does the job well enough. While ammonium sulphate may be a superior choice for efficacy in salting out, it will emit fumes of ammonia when sodium hydroxide or any similar strong base is added. Loveall has posted some links to principles of salting out and which salts are the most effective.




“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
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
Nordic traveller
#3342 Posted : 10/16/2021 1:16:58 PM
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Thanks, downwardsfromzero!

I'll probably experiment with different salt concentrations including no salt.
 
monomind
#3343 Posted : 10/24/2021 1:59:52 PM

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Greetings Nexians,

A couple of questions for the knowledgeable ones Smile

1. Is there a way to wash d-limonene from plant fats and other gunk so it can be reused many times ?
2. When performing hot pulls, what temperature should I have my soup and d-limo ?
( I use a sous-vide pot so can adjust the temperature accurately )

Thanks!
 
Dirty T
#3344 Posted : 10/24/2021 5:03:10 PM

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I know some people do an activated carbon wash with a lot of success on various solvents. I backsalt then calcium carbonate wash my Naptha and Xylene after every run. The Xylene has a tendency to retain more color but that's fine since I backsalt all Xylene pulls anyways. The Naphtha always comes out very light colored. I've been using the same NPS for a long time, no need to replace and honestly a tiny bit of color in the starting solvent has never translated to ugly crystals for me.

I do my Naphtha pulls at 55* C with a boiling water bath on the soup. I do Xylene at 90* C. I have done hotter and colder for both but these are the optimal spots in my experience (I don't worry about the bath temp, I also have a sous vide but don't use it for DMT). Hopefully someone can come along and give the proper temperature for D-Limonene or you could try searching "D-Limonene Heated Pulls". I get better results punching "my search text" + DMT Nexus into Google sometimes than I get with the engine here and have read others have similar experiences.
 
monomind
#3345 Posted : 10/24/2021 5:30:48 PM

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Dirty T wrote:
I know some people do an activated carbon wash with a lot of success on various solvents. I backsalt then calcium carbonate wash my Naptha and Xylene after every run. The Xylene has a tendency to retain more color but that's fine since I backsalt all Xylene pulls anyways. The Naphtha always comes out very light colored. I've been using the same NPS for a long time, no need to replace and honestly a tiny bit of color in the starting solvent has never translated to ugly crystals for me.



Thanks for your reply.
My chemistry knowledge is not much, so can I kindly ask that you elaborate a bit on the process ?
Also, as far as I understand, back-salting will not remove any fats etc into the the low ph medium.
It will pull dmt into it though, if it exists in the nps ( I perform that to clean up ACRB pulls )
Am I wrong on this ?

Thanks again Smile

 
Dirty T
#3346 Posted : 10/24/2021 7:07:34 PM

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Backsalting is very simple. You just drop your DMT laden NPS into an acidic mixture (I use acetic acid, distilled white vinegar diluted to 5% acidity. I don't dilute with water. I use a Pyur 500ml bottle with 300ml acetic acid and backsalt 150ml NPS at a time. I place on a scientific hot plate at 60 or 90 C depending on the NPS I am backsalting and set the stir function to 1250 rpm. I check after 30 minutes. When you pour the NPS into the acid it will immediately become cloudy. Once the NPS clears up and the acidic solution becomes cloudy it's finished and you can remove and replace the NPS until it's all clean)

Once you have backsalted all of your NPS you have to basify by pouring your acid into a larger container then diluting and adding base (dissolved in water) I move from a 500ml container to a 2L container and add 25g NaoH to 450ml distilled water, dissolve then add to the acid. I do this twice then add distilled water until the NPS is at the tapered part of the bottle. Then I add 100ml NPS and stir at 60* C at 1250 RPM) you can always check your progress by allowing it to settle overnight. (Today I woke up to a snow globe with a massive pile of orange crystals on the bottom of the bottle. I'm not convinced Naphtha will even pick it up but am pretty positive it's DMT, it all came from MHRB).

Do as many pulls as necessary to pick up the DMT from your basified 2l bottle.

After you have finished the entire backsalting process (now your NPS wil have a definite acidic smell and depending on the NPS may have some residual 'cloudiness' we remove both of those issues with this step) you can start cleaning with sodium carbonate wash. In a 1L jar Add 60g sodium carbonate to 750ml distilled water. Add NPS and stir on hot plate or shake vigorously. When it settles pipette the NPS off the top. You can repeat this 3 times. This process always leaves my Naphtha a very light color, my Xylene stays yellow but the cloudiness and acid smell go away and that's my main concern.
 
monomind
#3347 Posted : 10/24/2021 7:29:14 PM

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Thank you Dirty T...

That's a great answer! and very helpful to the process I am trying to execute.

Thumbs up
 
monomind
#3348 Posted : 10/26/2021 3:04:49 PM

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Dirty T wrote:
Backsalting is very simple. You just drop your DMT laden NPS into an acidic mixture (I use acetic acid, distilled white vinegar diluted to 5% acidity. I don't dilute with water. I use a Pyur 500ml bottle with 300ml acetic acid and backsalt 150ml NPS at a time.

If you don't mind me asking you another question:
Do you use the same 300ml acetic acid with multiple 150ml batches of nps, or each time its a fresh 300ml ( and then combine them I assume) ?

Dirty T wrote:

Once you have backsalted all of your NPS you have to basify by pouring your acid into a larger container then diluting and adding base (dissolved in water) I move from a 500ml container to a 2L container and add 25g NaoH to 450ml distilled water, dissolve then add to the acid. I do this twice then add distilled water until the NPS is at the tapered part of the bottle. Then I add 100ml NPS and stir at 60* C at 1250 RPM) you can always check your progress by allowing it to settle overnight. (Today I woke up to a snow globe with a massive pile of orange crystals on the bottom of the bottle. I'm not convinced Naphtha will even pick it up but am pretty positive it's DMT, it all came from MHRB).


I have 150ml of DMT rich NPS ( limonene ) altogether.
Any recommendation as to how much acetic acid I should use ?
And how much NaoH ?

Thanks again !

P.s.
My 150ml of NPS has less than 1g of DMT in it




 
downwardsfromzero
#3349 Posted : 10/26/2021 4:56:50 PM

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monomind wrote:
I have 150ml of DMT rich NPS ( limonene ) altogether.
Any recommendation as to how much acetic acid I should use ?
And how much NaoH ?

Thanks again !

P.s.
My 150ml of NPS has less than 1g of DMT in it

Divide MW of acetic acid [C2H4O2 = 60] by MW of DMT [C12H14N2 = 186] to get the amount in grams of pure acetic acid that will react with one gram of DMT. If using 5% w/v vinegar, multiply the result from the first calculation by [1/0.05 =] 20 to get the volume of vinegar that will react with one gram of DMT:

(60/186)*20 = 200/31 ~= 6.45 mL

Divide MW of sodium hydroxide [NaOH = 40] by MW of DMT [C12H14N2 = 186] to get the amount in grams of sodium hydroxide that will neutralise the 6.45 mL of vinegar, or of course freebase the resulting amount of DMT acetate solution:

[This is easy, because it's 2/3 of the result from the very first calculation, or 1/30 of the volume of vinegar]
40/186 = 0.215 g or 215 mg [6.45/30 = 0.215]

In practice, solid NaOH will be less than 100% pure through absorption of CO2 and water from the atmosphere.


Clearly these tiny amounts are best measured volumetrically after making up a standard solution of NaOH. You'll be best off using larger volumes of both the vinegar and the lye for ease of handling. You might want to consider using diluted vinegar so that you're not pointlessly creating excess sodium acetate.




“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
 
monomind
#3350 Posted : 10/27/2021 10:28:07 AM

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downwardsfromzero wrote:

Divide MW of acetic acid [C2H4O2 = 60] by MW of DMT [C12H14N2 = 186] to get the amount in grams of pure acetic acid that will react with one gram of DMT. If using 5% w/v vinegar, multiply the result from the first calculation by [1/0.05 =] 20 to get the volume of vinegar that will react with one gram of DMT:

(60/186)*20 = 200/31 ~= 6.45 mL


Thanks for the informative answer!
If I understand correctly, then 6.45 mL is the minimum amount of acetic acid required to convert 1g dmt to salt form.
Correct ?
The vinegar solution will need to "touch" all parts of my NPS in order to do that so I assume using a larger volume of vinegar solution will be more efficient ( given also that I don't have a magnetic stirrer)

Whatever amount I use... will then need to be basified with NaoH - so I also don't want to use too much.
Maybe 1:1 NPS : Diluted Vinegar will be a good voluem to work with ?
Also, is one iteration of NPS-->Vinegar is enough ? or should I do multiple "pulls" ?

Thanks in advance!

 
Dirty T
#3351 Posted : 10/27/2021 6:06:52 PM

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You only have to put the NPS into the acid once, it will cloud up immediately as the DMT begins to crash out into the acid. When the reaction is finished the NPS will 'clear up' and the acid will become cloudy. No additional "pulls" are needed for this step. Before I used a hot plate I would use a hot water bath and just shake the ever living feces out of the bottle (I backsalt in 500ml PYUR borosillicate glass jars). The heat assists with the migration from the NPS to the low PH solution.
 
downwardsfromzero
#3352 Posted : 10/27/2021 6:23:30 PM

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monomind wrote:
If I understand correctly, then 6.45 mL is the minimum amount of acetic acid required to convert 1g dmt to salt form.
This is the volume of 5% acetic acid that you would use, to be clear.

You can dilute that down with distilled water to a more easily recoverable volume (6.45 mL being just over a teaspoonful), and/or after removing the vinegar you could perform a second pull using only distilled water which you then combine with the first vinegar pull - or even evaporate down to see if it was worth doing it at all.




“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
 
monomind
#3353 Posted : 10/28/2021 12:42:50 PM

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Dirty T wrote:
You only have to put the NPS into the acid once, it will cloud up immediately as the DMT begins to crash out into the acid. When the reaction is finished the NPS will 'clear up' and the acid will become cloudy. No additional "pulls" are needed for this step. Before I used a hot plate I would use a hot water bath and just shake the ever living feces out of the bottle (I backsalt in 500ml PYUR borosillicate glass jars). The heat assists with the migration from the NPS to the low PH solution.

Got it.
In my case its d-limonene from ACRB pulls and I used citric acid instead of vinegar ( just because it smells better Smile )
The d-limo contains also ACRB fats so I mixed it with a spoon rather than shake. Gentle emulsion still occurred, but I could easily break them with a spoon.
The acidic solution got cloudy, and it also smells faintly of oranges now so I assume it pulled more than just the alkaloids.

downwardsfromzero wrote:

after removing the vinegar you could perform a second pull using only distilled water which you then combine with the first vinegar pull - or even evaporate down to see if it was worth doing it at all.

Thanks, will give this a go!

 
Dirty T
#3354 Posted : 10/28/2021 5:32:55 PM

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My last backsalt from Xylene resulted in a pile of orange crystals on the bottom of the jar. Naphtha wouldn't pick them up. Xylene did and I still need to pull the Xylene out and evaporate to see what exactly it is. It came from MHRB so I would assume it's "jungle alkaloids" but it's a whole lot for the source amount. I'll report back once I've evaporated as to what it actually pulled.
 
downwardsfromzero
#3355 Posted : 10/29/2021 8:08:08 PM

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monomind wrote:

In my case its d-limonene from ACRB pulls and I used citric acid instead of vinegar ( just because it smells better Smile )
The d-limo contains also ACRB fats so I mixed it with a spoon rather than shake. Gentle emulsion still occurred, but I could easily break them with a spoon.
The acidic solution got cloudy, and it also smells faintly of oranges now so I assume it pulled more than just the alkaloids.

Citric acid does have some emulsifying properties so emulsions are more likely with it. Glad to hear it was easy to break the emulsion that you got.

Citric acid may or may not be responsible for pulling some of the limonene into the aqueous phase because of this emulsifying property. Limonene is, however, notably more reactive than many NPSs. It forms oxidation products which can also smell fairly citrussy and which furthermore have a greater tendency to dissolve at least slightly into the aqueous phase.

Recrystallizing the DMT citrate from boiling anhydrous IPA should go some way towards clearing up this odour if it proves to be excessive. In my view, excessive contamination from limonene oxidation products could adversely affect the shelf life of the product. This may or may not be an issue depending on how quickly you end up using it.




“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
 
monomind
#3356 Posted : 10/31/2021 12:41:21 PM

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downwardsfromzero wrote:

Citric acid does have some emulsifying properties so emulsions are more likely with it. Glad to hear it was easy to break the emulsion that you got.

Citric acid may or may not be responsible for pulling some of the limonene into the aqueous phase because of this emulsifying property. Limonene is, however, notably more reactive than many NPSs. It forms oxidation products which can also smell fairly citrussy and which furthermore have a greater tendency to dissolve at least slightly into the aqueous phase.

Recrystallizing the DMT citrate from boiling anhydrous IPA should go some way towards clearing up this odour if it proves to be excessive. In my view, excessive contamination from limonene oxidation products could adversely affect the shelf life of the product. This may or may not be an issue depending on how quickly you end up using it.

Thank you downwardfromzero, your posts are very informative.
My citrate stage was just for cleanup. It was basified again, pulled with d-limo and then added FASI to crash out fumarate.
So I believe the back-salting I did was totally redundant in this context given I planned to end up with dmt fumarate.
Live and learn Smile

Just in passing...I put the FASI in paper filter above the d-limo so its dripping very slowly.
There is a cloud building up in the d-limo which seems to be travelling down in "one block".
Once it reaches the bottom of the jar ( hope it will indeed) I will add more FASI to see if more clouds are formed.
 
The Gnome
#3357 Posted : 11/23/2021 8:28:07 AM

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Hello, I havent gotten MHRB in over a decade! Ive heard stories of low yields with more current root bark. In the US, whats the average percent yield one should expect from a Domestic Vendor?
 
Scatterday
#3358 Posted : 11/26/2021 7:37:45 AM
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For the last few hours I've been researching Acacia extractions but I'm still left with some questions and wanted clarifications on a few things.

Are A/B extractions still best for Acacia root bark specifically Aanprb and would you need to defat?

Are ACRB and Aanprb interchangable in an extraction, Could someone use a different type of Acacia bark in place of the confusa that's rich in dmt?

Is there a guide on how to scale up or down extractions?

Is heat bad for Aanprb/Acacia, If so why do so many teks boil the bark. How much heat is too much?

Where could someone start if they wanted to design their own tek?
 
Tony6Strings
#3359 Posted : 11/26/2021 9:16:53 AM

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Anything written for acrb should be interchangable with any other acacia root bark. For acacia confusa (and mimosa) I use a standard A/B: powder bark, three acetic boils (cover with water and healthy splash of vinegar, bring to rolling boil, turn down to low and simmer for 30 minutes, pour through cloth filter, repeat entire process twice more with fresh water and vinegar each time on same bark). Tea is collected and reduced to fit in 1000ml Erlenmeyer or other appropriate vessel. Base with NaOH, I use 1/4 of starting bark weight, so, 25 grams lye for tea made from 100 grams root bark. Pull with new vm&p naphtha 100 ml at a time. Freeze precipitate.

There are other teks for phylodes, and some people like to defat before basing or mini AB or re-x for goo issues. As written with no additional steps, I have used this Tek to produce everything from snow white crystal fluff to red wax and everything in between.
https://www.dmt-nexus.me...aspx?g=posts&t=96736

Depends on your acacia bark and maybe how hot/humid it is in your place atm. I'm going to try again now for more white crystal now that it has cooled down.
olympus mon wrote:
You need to hit it with intention to get where you want to be!

"Good and evil lay side by side as electric love penetrates the sky..." -Hendrix

"We have arrived at truth, and now we find truth is a mystery- a play of joy, creation, and energy. This is source. This is the mystic touchstone that heals and renews. This is the beginning again. This is entheogenic." -Nicholas Sand
 
downwardsfromzero
#3360 Posted : 11/26/2021 2:00:16 PM

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Scatterday wrote:
Is there a guide on how to scale up or down extractions?
It's a simple fact of life that larger extractions become more cumbersome to handle. It's best to stick to the amounts cited in the usual recipes until you've become more experienced in extracting.

There are some arithmetical limitations that arise when increasing the size of an extraction. One of the most important to consider is the difference in scaling between surface area and volume. Area scales as the second power whereas volume scales as the third power, so liquid/liquid extraction equations do not scale linearly. They become less efficient as they get larger and at some point it necessitates the use of specialised equipment.

Another thing is heat transfer through the brewing phase. Scorching is more likely to occur while heating a large pan of sludge, both because of the area/volume scaling factors involved and that a thick layer of bark powder will tend to act as an insulator. Brewers and distillers typically use a kettle that can be heated through the sides rather than the base in order to minimise burning at the bottom of the vessel.

Please also take this information into account when deciding how large your extraction should be!




“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
 
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