Near full efficiency extraction

[1ce]

This isn't a tek, it's just an observation journal from a few extractions. It uses laboratory equipment and is not meant for beginners. Some practices and methods may not be safe, suitable, and feasable for many here. But that's not the point.

50g bark is weighed out and measured, then ran through a food processor 2 times, and a coffee blender once. 500ml distilled water is boiled and enough citric acid is added to bring the ph to 2-3.

50g powdered mhrb is added to a 1000mL round bottom flask, 500mL citric acid solution is added, and finally, a 1" magnetic stirbar is added. The mixture is brought to a gentle boil at a heavy spin and left for 12-24 hours at reflux conditions.

The temperature of the mixture is brought down to 55C and 25ml VM&P is added. This is allowed to mix for 1 hour, reflux conditions are kept.

The mixture is poured out into a büchner funnel and filtered off into a 500ml side-arm flask. This is poured into a 1000mL beaker, and boiled down to 350mL. 35g NaOH is added to 150mL and added to the 350mL acidic solution. They are intimately mixed and ph is brought up to about 13.

The beaker is placed in a refrigerator and brought down to 20C. The solution is added to a 1000mL round bottom flask, 50mL methylene trichloride is added, and a 300mm alihn condenser is affixed so that I don't loose any solvent from evaporation. This is stirred vigorously for 1 to 1.5 hours. Then the mixture is poured into a 1000mL separatory funnel and allowed to separate. The chloroform is drained into a 250mL round bottom flask and evaporated under reduced pressure to avoid oxidation and to allow for solvent recovery.

150mL anhydrous dimethyl keytone is added to the flask and allowed to dissolve the DMT and other alkaloids from the flask, another 150ml of fumaric acid saturated acetone is added and DMTZ fumarate is crashed out. The DMK is evaporated with a vacuum to avoid oxidation and reduce fumes.

Boiling water is added dropwise to the acid until dissolved completely. It is then based with sodium carbonate and pulled with 50% by volume, boiling heptane. This is allowed to cool and evaporate (without a fan) until crystal formations begin to appear. A lid is placed over the container, and placed in a refrigerator after a few hours.

After a few hours in the refrigerator, (2-3) it is added in the freezer, and harvested later.

----- NoTeS -----

Multiple pulls, and acid boils have not yielded any additional spice. I'm assuming my efficiency is quite high, the remaining spice is somehow destroyed, or there is so little that I overshoot the solvent when collected. However this would be evidenced when the methylene trichloride is fully evaporated, however no residue is left behind.


I try to defat at a temperature that facilitates the transfer of fats and oils. I try to keep the solubility of the naptha no higher than this point. Just incase I've lost anyproduct from a heated was, I've kept all of my naptha from the washes.

 

[Jees]

What a nice hobby you have.
yield % ?

 

[concombres]

Looks like some top quality spice 1ce :d
Every time i see you post an extraction technique it makes me wish i had access to a nice glassware collection & lab grade solvents.

On a side note, how have you not been promoted to full membership yet?
I just noticed that. I'd have thought you've been here for years already from the content of your posts.

 

[benzyme]

It uses laboratory equipment...

50g bark is weighed out and measured, then ran through a food processor 2 times, and a coffee blender once.

what? no rotor-stator homogenizer?

 

[lewinii]

what? no rotor-stator homogenizer?

:lol:

 

[downwardsfromzero]

methylene trichloride is added

Is that dichloromethane (= methylene dichloride) or trichloromethane (= chloroform)?

Note that chlorinated solvents such as these have been shown to form small amounts of impurities by reacting with the alkaloids.(There's a ref. somewhere, but beyond me right now.) Recrystallisation should take care of this.

 

[1ce]

methylene trichloride is added

Is that dichloromethane (= methylene dichloride) or trichloromethane (= chloroform)?

Note that chlorinated solvents such as these have been shown to form small amounts of impurities by reacting with the alkaloids.(There's a ref. somewhere, but beyond me right now.) Recrystallisation should take care of this.

Hello there! Thank-you for the sound advice! I have a concern however.. it seems as though you might have misplaced your post. I do believe you meant to be here instead.

Sincerely, 1ce.

 

[downwardsfromzero]

You're not the only person reading your posts, you know. You're coming across as a bit arrogant as time passes. That is unwarranted.

Are clarifications deemed irrelevant in your world of self-mastery?

 

[1ce]

You're not the only person reading your posts, you know. You're coming across as a bit arrogant as time passes. That is unwarranted.

Are clarifications deemed irrelevant in your world of self-mastery?

Google: methylene trichloride

TCM will not ruin your extraction, it has been discussed throughout the forums, especially in recent passage. This is the advanced chemistry section of the forums, and chloroform use is standard practice for use as an extraction solvent. I figured you may not have known that so I linked you to a suitible place: Basic chemistry. Extractions are commonplace, and so are chlorinated solvents.

Regards, 1ce

 

[downwardsfromzero]

OK, so you're an industrial chemist. Nomenclature might not be your strong point

Beautiful crystals, btw:roll:

 

[1ce]

OK, so you're an industrial chemist. Nomenclature might not be your strong point

I am not an industrial chemist. Solvent choice might not be your strong point as indicative of your post history.

 

[downwardsfromzero]

Still, that's the first time in 30 years of chemistry I've ever seen/heard chloroform refered to as 'methylene trichloride'. That's why I asked.

Solvent choice might not be your strong point as indicative of your post history.

I'm not a fan of chlorinated solvents for a number of reasons beyond their immediate utility as solvents.

What else might you be referring to?

 

[1ce]

Still, that's the first time in 30 years of chemistry I've ever seen/heard chloroform refered to as 'methylene trichloride'. That's why I asked.

Solvent choice might not be your strong point as indicative of your post history.

I'm not a fan of chlorinated solvents for a number of reasons beyond their immediate utility as solvents.

What else might you be referring to?

Advising people in the welcome area to use diethyl ether might have gone a bit too far.

 

[downwardsfromzero]

I seem to recall suggesting that wouldn't be a good idea. I'll just go check and edit it if it is as you say, as that would indeed be ridiculous. Anon.

 

[downwardsfromzero]

Sorry to go on and thread-jack but in the interests of fairness:
Here are my most recent posts regarding ether in the welcome area:
12th August 2014

Ether is quite dangerous. It has a very low boiling point compared to heptane, making it extremely flammable. Also, it slowly forms explosive peroxides which can make evaporation of significant quantities quite hazardous. Not to mention its anaesthetic properties.

08 January 2015

mixed it with an equal amount of Sodium(Bi)Carbonate

If you used bicarbonate there won't be very much freebase for the ether to pick up at all. You should at least use sodium carbonate - washing soda. Do you get the difference between this and sodium bicarbonate - baking soda?

Do an evap test on a small amount of the ether to see if it's picked anything up.

As far as evaporating ether goes - ummm... that looks like an awful lot of ether to evaporate. That would seem terribly wasteful. Are you trying to blow yourself up?? And you do know of ether's tendency to form explosive peroxides, don't you?

Why are you messing around with an untested technique involving an extremely flammable solvent, anyhow? Please be careful. You don't want to end up in the newspaper (and/or the morgue) for the wrong reasons.

(emphasis added)

10 January 2015 01:51:02

Could I add salt to the water and increase ionic strength to prevent the ether dissolving in the water and fuck up my extraction?

Adding salt will help. You don't really want too much ether dissolving in the water. It's not about the ether dissolving in the water.

Should I rather just change solvent because ether is not good enough for a/b DMT extraction?

I'd save the ether for huffing. But that's just me being degenerate. We don't hear much about ether extractions round here so it might be interesting. Just so long as you stay safe.

(emphasis added)

OK, not an out-and-out admonishment against ether usage, and I'll admit to being flippant about the huffing. Don't huff ether, that's stupid and dangerous.

10 January 2015 03:08:36

wrote:
We don't hear about ether (diethyl? ) extractions here because it's not safe in a home extraction setting. Ether can have a real nasty temperment.[...]

Thanks for saying, I already mentioned this to him (ektor) elsewhere.

PS, it was ektor says he's an industrial chemist. Sorry, I got you two mixed up!

 

[1ce]

Fair enough. Diethyl ether has very dense fumes. Dense enough to almost be treated like a liquid, and rediculously flammable. The kind of flammable that is easily exploited by a home, with all those pilot lights, wall outlets, A/C telephones, tvs, spark producing appliances.. any one of these things could start a very violent fire. Let's ice the cake with that bottle of ether detonating in your face.

Ether isn't a bad chemical, I use it periodically as I need it. But it has a very ill temperment; and requires a proper 'ether safe' work space. The advanced extraction chemistry section is about the only proper place for ether talk, and since it's risks outweigh the the benefits for a humble DMT extraction it almost plays no role here either.

Having synthed and worked with nitroglycerin and diethyl ether both on many occasions, I hold the opinion that handling nitroglycerin is considerably safer than diethyl ether. I don't recomend either, at least not on these forums.