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[Updated] My A/B tutorial, pics to come soon :) Options
 
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#1 Posted : 9/13/2016 12:42:24 AM
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Hi fellow Nexians!

As promised, I've updated and changed my thread so that it's not full of crap

Before we begin please note that I intend to add pictures as I can get them, I will upload hi-res images and videos of anything that might be helpful to clear any misunderstandings up and help streamline this for us everyday Nexians!

I put together a tutorial mostly based on Earthwalker's 100g ACRB Tek and some other relevant information from Cyb's tek and the community as well as going through the principles of alkaloid extraction, and after performing my first extraction on this slightly modified tutorial I decided to post it after I had a successful yield and put to rest any doubts I had on my ability to perform this!

Here we go!


PREFACE:

If you would like to have a clearer Understanding of alkaloid extraction and any principles going on here, I'd like to direct you to the few following links
(Insert links)...

Here is a somewhat simplified Explanation of an A/B (acid - base) extraction. (I have modified this extract a little bit from the source below to reflect DMT, although this process still applies to other alkaloid or drugs etc.)

Most drugs have an amine group. This is a -NH2 attached to the molecule somewhere. NH3 is a 'base' (accepts protons from acids easily) so this makes DMT a 'base' also. Hence the name freebase. When you make the drug, it starts out in the freebase form, which is quite often an oil. What happens when you react an acid and a base? You get a salt. So when you take your freebase DMT and react it with an acid, you get a DMT salt (When DMT is dissolved in hydrochloric acid (HCl), it forms DMT hydrochloride, when it is dissolved in acetic acid (CH3COOH), it forms DMT acetate).

Salts are usually crystalline solids rather than oils or waxy solids, which is why they are so popular with drugs, it makes them easier to handle, and the drug properties are not changed. DMT salts also store very well with a longer shelf life than freebase DMT which is also very important to consider if you plan on holding onto it for a long period of time.

Freebases and salts usually have drastically different properties. An important property is that freebases are usually soluble in non-polar solvents (such as toluene and (hot) naphtha), and not soluble in polar solvents such as water. The salts are usually the opposite, soluble in water, but not toluene etc. This is how acid/base extractions (A/B) work.

You can basify your molecule with NaOH (lye) to form the freebase, which is not soluble in water, but it will dissolve in a non polar solvent. So you add your non-polar solvent and the freebase goes in to it (a lot faster if you allow the solvent to circulate through the solution instead of waiting for the freebase to float up to it).
Once you have freebase DMT in your non-polar you could wash the non-polar solvent with water to get rid of any non-freebase drug material (such as excess lye) and the water will not remove any of your freebase.

However!

Since evaporating water sucks, and quite often leaves behind impurities, it is much more desirable to recover your freebase in a non-polar solvent, which are quite handy as they evaporate much much faster due to their very low boiling point.

It is worth mentioning that cold alcohol doesn't dissolve crystals very well, which is why these teks opt for hot alcohol(or naptha or Shellite in our circumstances) it is better to (safely!) heat our non-polar solvent prior to adding to the solution and then pipette into a suitable container, cool down the solvent and the crystals will come back out (recrystallize). The slower you cool the solvent, the bigger the crystals are. The bigger the crystals are, the fewer impurities will be trapped inside of them, and the purer your product will be. So big crystals = pure crystals (usually).

One good way for ensuring that your alcohol cools down nice and slow is to boil some water and take it off of the heat. Then put your container with hot solvent and dissolved crystals in the hot water bath (being sure not to get any water into the solvent), cover the container, and let it cool down to room temperature. Then you can put the container with your solvent in the refridgerator to cool more. Then into the freezer to cool more. After this stage there is usually still a little bit of product left in the naptha, we can either evaporate the remaining solvent to nothing which results in 100% recovery, or we can decant and Pipette the solvent for future extractions. Either way is up to you, just remember that if you recover the solvent you may leave some DMT behind, albeit not very much.

Source: https://drugs-forum.com/...t/rextal.a-b.basics.html

so with this out of the way lets move on to the tutorial!


This tutorial is designed for 100g of Acacia Confusa Root bark, I am not sure on scalability of this tek, i would prefer not to attempt wasting materials to test it at this stage becuase I would have to experiment with larger volumes and times and temperatures which I am just not prepared to do unless others can verify this can be scaled without compromising on yield, which would probably involve side-by-side comparisons.

Ingredients:
-100g Powdered ACRB
-1.0L of Acid stock solution
-0.5L of Basic stock solution
-1.0L of saline stock solution
(4.0L of De-ionised/distilled water in total, including topping up the volume of the solutions)
-1.0L bottle of Shellite (non-polar Solvent) -(~50mL Per Pull)

Materials:
-2L Glass/HDPE Bottle w/secure lid (for primary A-B)
-1L glass bottle w/secure Lid (for secondary A-B)
-3x 1.0L or larger HDPE bottles for stock solution (distilled water containers will be adequate as long as they have the 2 symbol in the recycle image)
-at least 1 Saucepan for waterbath
-2-3 glass jars with lids
-Digital Scale
-Glass measuring jug
-Turkey baster
-1x large ovenproof Glass Dish (for final freeze precipitation)

(Optional materials)
-Thermometer
-pipette/syringe
-Funnel
-Digital pH. Meter/pH. Test strips

*Prior to the extraction you should prepare yourself several Litres of stock solution, these will help streamline the process and save valuable time when needed!

*Saline stock*
-For every 1L of Distilled water, dissolve 80g of table salt by boiling to aid in dissolving
*Acid stock*
-For every 1L of Distilled water add 120mL of White vinegar (this is exactly 1/2 cup)

*Basic stock*
- For every 1L of Distilled water add 200g of Sodium hydroxide.

*WARNING* This is a Very high amount of Sodium hydroxide and caution must be taken!
If you are doing this the first time, take your time and take note of the thermal reaction that takes place, colder water would be safer to allow for a buffer of temperature that can be more manageable, and please do this in glass and not in plastic as there is high risk that the plastic will deform and possibly melt!
Always remember to add NaOH to water (and very slowly and carefully!) and never water to NaOH!

Here is what happens when you add NaOH to boiling water https://youtu.be/dZb_wPJivpo

Method



Stage 1: Acid to Base

-Bring 1/2 a Large pot of tap water to the boil and then reduce to the lowest temperate setting To keep it below a simmer.

-In a 2 Litre Glass bottle place your Powdered material and 500mL of your Acid stock solution and combine well so there are no dry clumps and is of even consistency.

-Place the bottle in your hot waterbath for a minimum of 1.5 hrs. You may notice when you lift the bottle out of the waterbath that there will be some layers that have separated so give this a good swirl every few minutes to mix well.

-Using a funnel pour the 1L of saline stock solution into the 2L Bottle containing the acidic solution. Give this a quick swirl to combine the two.

-Add 300mL of Basic stock solution to the 2L bottle, on contact the solution will turn a deep Red/purple close to black. At this point you can add a small amount of Distilled water to increase the volume but leave enough room for your solvent so you will be pipetting from the neck of the bottle. This is a huge advantage as there is less surface area and you will have less chance of sucking up any of the oils and Basified liquid.

-Swirl briefly to make sure all the solutions have combined and place the bottle back into the saucepan for a minimum of 2 hours, remember to swirl the bottle occasionally to mix up any sediment



Stage 2: Solvent pull

-Fill a glass jar with Shellite/Naptha and place the lid on just a bit loose to allow any release of pressure build up.

-Remove our bottle from the saucepan and place in on a towel, bring our water just barely to a simmer and then remove it from the heat source. Lower your glass jar of solvent into the water being careful not to let the jar tip over (if you have a smaller saucepan use this, alternatively if there is too much water, you can pour some out) you may observe the solvent begin to boil, at this point remove it from the saucepan.

-Using your Turkey baster, extract ~50mL of the hot solvent and add it to your 2L bottle of your solution. (It is advisable to hold your jar Close to the mouth of the bottle as the turkey baster will drip and squirt).

-Mix well by turning over end to end and swirling the bottle with the lid on tight to aid in the migration of the DMT particles into the solvent for 1 minute, ensuring that you pop the lid after a few seconds to release any build up of pressure.

-place the bottle back in the saucepan and allow the Solvent to separate from the solution, this may take several minutes, and if your base solution is cool the separation may take longer.

-Pipette the solvent out of the solution and place into a jar, making sure to avoid sucking up any of the oils and Basified solution (Even if you do, the secondary A-B will clean this out). Close the lid of the jar and put it aside. As you suck the solvent out, you will notice it will instantly cloud up, this is the DMT precipitating out due to the drop in temperature. This is completely normal.

-repeat this stage as many times as you feel necessary, many teks opt for 5-6 pulls. You might notice that the pulls stop becoming cloudy and that may be your indication that there is very little dmt left in the solution, If you wish to evaluate the solution, place the final pull into a separate smaller jar and run a freeze precipitation/evaporate separately.



Stage 3: Secondary A-B (Mini A-B/Clean up/Re-X)

-Add the remaining 500mL of acid stock solution we prepared earlier to a 1L bottle with a thin long neck (one that will allow our Turkey baster to fit)

-Pour our Shellite pulls from the previous stage into the acidic solution and shake for up to 10 minutes (Depending on the level of oils and fats present in your Shellite pulls you may have to avoid shaking. Allow the layers to separate which may take several minutes. You may notice that your Shellite which was milky and perhaps discoloured is now almost clear, while your acid stock which was clear is now cloudy! This is an indication that the DMT Freebase has migrated into the acid and turned into a DMT Salt.

-Pipette out the Shellite layer and put it in a jar, the solvent has no further use at this stage and can be either discarded or reused for further extractions. This time we are keeping the acidic solution in the bottle which contains the DMT.

-Add the remaining 200ml of our Basic stock solution to the 1L bottle. The solution will turn a milky colour on contact with the the base stock. This is the DMT precipitating out of the acidic solution and migrating back towards the basic solution! Add some distilled water if needed leaving enough room for 50mL of hot Shellite.

-Add 50mL of hot Shellite and With the lid on firm, shake the solution several times, stopping inbetween shakes to release any build up of pressure, then place the bottle in the saucepan with the lid loose for a few minutes until the shellite layer separates and all the bubbles and any oils remaining settle, pipette out the solvent layer and place into a large glass dish. Continue this step 5-6 times or until the solution is clear or not giving out any more DMT.



Stage 4: Evaporate/Freeze precipitation

-At this point you have two options:

1: Place a lid on the dish or cover with cling wrap, place it in a safe location and allow it to cool to room temperature, (I left it overnight) then place into the freezer for 24 hours.

After removing from the freezer immediately pour off the shellite into a jar for future extractions, being careful not to pour out any crystals. Don't let the solvent warm up or the DMT will start to re-dissolve. Place the dish under a fan and air dry until the solvent is completely evaporated and there is no longer any smell of Shellite! This can take an hour or more

2: Place the open dish somewhere well ventilated and away from any dust and foreign material and allow to evaporate completely.


Congratulations you now have freebase DMT, photos will be up soon and text editing, thanks for watching Smile
 

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corpus callosum
#2 Posted : 9/13/2016 2:43:41 AM

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Astro84 wrote:

It is worth mentioning that cold alcohol doesn't dissolve crystals very well, which is why these teks opt for boiling/hot alcohol (or naptha in our circumstances) it is better to (safely!) boil our non-polar solvent prior to adding to the solution and then pipette into a suitable container, cool down the solvent and the crystals will come back out (recrystallize).


"Boiling" non-polar solvents conjures up some hazardous visions in my mind, fraught with the risk of fire and explosions. Because these solvents typically have a much lower boiling point than say water, it is sufficient (and so much safer) to use a water bath to heat the solvent rather than attempting to apply direct heat via a flame to a container containing such a solvent.
I am paranoid of my brain. It thinks all the time, even when I'm asleep. My thoughts assail me. Murderous lechers they are. Thought is the assassin of thought. Like a man stabbing himself with one hand while the other hand tries to stop the blade. Like an explosion that destroys the detonator. I am paranoid of my brain. It makes me unsettled and ill at ease. Makes me chase my tail, freezes my eyes and shuts me down. Watches me. Eats my head. It destroys me.

 
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#3 Posted : 9/13/2016 3:31:32 AM
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corpus callosum wrote:

"Boiling" non-polar solvents conjures up some hazardous visions in my mind, fraught with the risk of fire and explosions. Because these solvents typically have a much lower boiling point than say water, it is sufficient (and so much safer) to use a water bath to heat the solvent rather than attempting to apply direct heat via a flame to a container containing such a solvent.


Yes of course I am completely aware of the serious hazards of directly heating a vaporous solvent that can ignite quite easy, I'm simply extracing this info from the provided link, I will make the required adjustment, obviouslty these are all under very controlled conditions which 99% of us do not have!

Thanks for pointing that our Corpus! Smile
 
Psilosopher?
#4 Posted : 9/13/2016 5:22:46 AM

Don't Panic

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Astro84 wrote:
I would like to contribute a thorough tutorial to the community that all can understand that isn't overly complicated to the newbies, clean and easy to read, with plenty of helpful hints and references that take you out of the tutorial, without cluttering the whole thing up.


I've attempted something similar.

https://www.dmt-nexus.me...aspx?g=posts&t=70899

And here's my unfinished tek comparison.

https://www.dmt-nexus.me...aspx?g=posts&t=68188


Hopefully you will find this useful.
"A common mistake that people make when trying to design something completely foolproof is to underestimate the ingenuity of complete fools."
 
DELETED_USER00002
#5 Posted : 9/13/2016 10:34:10 AM
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Thabks Bodhisativa, I recall reading this a while ago, it's good to revisit this thread and refresh the mind, I'll take in as much as I can once I got some time out to focus Smile
 
FLeP
#6 Posted : 9/14/2016 2:04:51 AM

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Personally I would get an extraction or two (or 1002) before attempting a tutorial.
 
Psilosopher?
#7 Posted : 9/14/2016 2:16:24 AM

Don't Panic

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FLeP wrote:
Personally I would get an extraction or two (or 1002) before attempting a tutorial.


This. I had innumerable failures before I had my first trip, let alone writing a methodology.
"A common mistake that people make when trying to design something completely foolproof is to underestimate the ingenuity of complete fools."
 
DELETED_USER00002
#8 Posted : 9/19/2016 6:57:06 AM
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I definitely intend to perform some A-B extractions before posting the tutorial, but more to the point I'm not writing a fresh new tutorial, this was more to follow for myself and another to follow based on the 100g acrb tek but easier to read (for me at least) and if it goes well I'll upload with pics
 
some one
#9 Posted : 9/19/2016 11:50:22 AM

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This is my newbe friendly dmt extraction tutorial which I hope sums up most info on dmt-nexus:
https://www.dmt-nexus.me...&m=418376#post418376

Personally I'm more the practical type, so left all the theoretical chemical background knowledge out.. That just complicates stuff further if you're just starting out and can better be left for a phase of curiosity at a later stage. But that's just me Pleased

Quote:
Personally I would get an extraction or two (or 1002) before attempting a tutorial.

I second this. Best of luck with your first extraction!
some = one | here = some | there = one
 
DELETED_USER00002
#10 Posted : 9/20/2016 3:08:36 PM
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Yea at first I wanted to know the steps only, just to get the job done. But that left a lot of unanswered questions I had in my mind, especially about why these reactions occur and how to make them more fruitful and so i became more curious about the process and ended up researching much more information to help me understand, which I'm sure there are some of you that don't want to know, but at least (in theory) i have an understanding of what to expect. And I am curious by nature and can grasp these things quite well.

Now with that out of the way I was wondering in regards to acidic and basic solutions, can I make a large quantity of a each to use later on so that I can not waste time on the day of the extraction, will these solutions store well? Do they at all settle and need agitation, or do they decay over time and is best made as necessary?
 
DELETED_USER00002
#11 Posted : 9/20/2016 5:00:02 PM
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some one wrote:
This is my newbe friendly dmt extraction tutorial which I hope sums up most info on dmt-nexus:
https://www.dmt-nexus.me...&m=418376#post418376

Personally I'm more the practical type, so left all the theoretical chemical background knowledge out.. That just complicates stuff further if you're just starting out and can better be left for a phase of curiosity at a later stage. But that's just me Pleased

Quote:
Personally I would get an extraction or two (or 1002) before attempting a tutorial.

I second this. Best of luck with your first extraction!


Wow dude, definately done the hard yarns there! Almost defeats the purpose of me writing a tutorial haha
 
Psilosopher?
#12 Posted : 9/21/2016 4:23:50 AM

Don't Panic

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Astro84 wrote:
Now with that out of the way I was wondering in regards to acidic and basic solutions, can I make a large quantity of a each to use later on so that I can not waste time on the day of the extraction, will these solutions store well? Do they at all settle and need agitation, or do they decay over time and is best made as necessary?


What you're asking is making stock solution. Not only is it not safe, but I highly recommend it. I have a section on making stock solution for any volume. It should be in the extraction section of my guide.
"A common mistake that people make when trying to design something completely foolproof is to underestimate the ingenuity of complete fools."
 
DELETED_USER00002
#13 Posted : 9/23/2016 2:39:25 AM
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Im blown away at the volume of the information you have in your thread Bodhisativa! I'll be doing a whole lot of reading today! thanks for the clarification, I'll get on to it Smile
 
DELETED_USER00002
#14 Posted : 9/23/2016 7:53:42 AM
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Just for some further clarification regarding the NaOH solution, Bodhisativa in your thread you describe using 80g per 1000ml of water, where as Earthwalker says to use 50-60g for 300mL, which is close to double your recommendation, and then in the clean up stages he uses 50g to 200ml water which becomes 2.5x your recommendation.

Is there a benefit of having a stronger base and a stronger acid for an extraction? Do these make for a higher yield? what's to stop me from making it (for arguments sake) 100g of NaOH per L? Is it more to do with constantly finding the balance by adding more and more stock to the solution? Meaning you run out of space or are there other factors at play?
 
Psilosopher?
#15 Posted : 9/23/2016 8:09:07 AM

Don't Panic

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Astro84 wrote:
Just for some further clarification regarding the NaOH solution, Bodhisativa in your thread you describe using 80g per 1000ml of water, where as Earthwalker says to use 50-60g for 300mL, which is close to double your recommendation, and then in the clean up stages he uses 50g to 200ml water which becomes 2.5x your recommendation.

Is there a benefit of having a stronger base and a stronger acid for an extraction? Do these make for a higher yield? what's to stop me from making it (for arguments sake) 100g of NaOH per L? Is it more to do with constantly finding the balance by adding more and more stock to the solution? Meaning you run out of space or are there other factors at play?


As long as the overall pH of the basified extraction is around 12, then it's all good. You could make really strong basic solution, but it just becomes more of a hazard, so there's no point. Initially, I was using 200 g of NaOH per litre.

When I did a titration of my stock acid solution, only a tiny amount of base was required of my stock base solution.


This is basically what I did.

Bodhisativa wrote:
some one wrote:
Nice find, something like that yes. However, uhm, I meant calculations with weights in mg instead of mol/vol. To use that site you need to do additional hand calculations and know what you're doing to be able to calculate the pH when you add 50g NaOH to 750ml water..

Update: according to the link 0.1 mole/liter of NaOH = pH 13. I thought pH 13 is enough to covert dmt salt to freebase.
0.1 mole = 4 gram. So for 800ml of water only 3.2 gram NaOH needs to be added to get pH 13.
But you are using 200ml of 200g/liter concentration in 800ml liquid = 40g (1.25mole/liter = pH 14.10).
This is what all teks are using (around 50g bark). Something is not right..

Also, in the OP you didn't explain (calculate) why you want 5M of NaOH.


Ah yeah, I didn't calculate why I needed 5M of NaOH. I just used that quantity to guarantee complete neutralisation. A bit overkill. Although this method works and gives plenty of spice, it is very wasteful of NaOH. I was in a bit of a rush with life in general when I wrote that part. I was planning on doing a titration to find out the optimal amount of NaOH required. I'll do just that, and edit the guide.

However, the MAX ION tek uses this:

4. Dissolve apprx 40g of NaOH (Lye) in a minimal amount of COOL filtered water (approx 100ml) and add to the acidic/saline mix.
A pH of 12+ is desired, so add more if necessary.



EDIT: I did the titration. I used 500ml of my stock solution HCl, and titrated against my stock solution of NaOH. HCl is 0.001M and NaOH is 5M.

Within 3mL of NaOH, the equivalence point was reached. At 5mL, the pH was 11. At 10mL the pH plateaud at 12, but I'm using a crappy pool pH meter. The guide has bee edited.


"A common mistake that people make when trying to design something completely foolproof is to underestimate the ingenuity of complete fools."
 
 
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