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official extraction help thread

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Right so my friend attempted his first extraction yesterday using mhrb. He followed q21q21's tek 2 and freeze precipitated the solvent. Took it out after about 15 hours. I could see some xtals in the jar forming and i thought there were much more on the sides of the jar, but this turned out to just be ice (i think).

he filtered the naptha (approximately 80-100ml ) through a coffee filter and didnt get anything,
But, the solvent is very cloudy. He assumes something might have gone, wrong or did he just not allow enough time for the xtals to form?

For now, he has put the solution back into the bark mix for the time being. He plans to wait a while till it returns to room temperature, then warm it up again and try freezing again, but this time for longer unless anyone has any other ideas/solutions?

any help appreciated :)
 
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So eventually , after combining an additional pull which was evaporated down first, before being put in the freezer, the 'white stuff' did start to appear around the jar which had been left for around 20 hours.

The solvent was filtered out, and the xtals were put onto a glass dish, which then started to melt within a minute or 2. I left this to evaporate, thinking that the solvent would leave the xtals on the dish but it's pretty much all gone now with nothing left behind.

Fortunately, only 100g of mhrb was used for this first extraction attempt, and the remaining pulled naphtha was put back into the bottle of unused naphtha. So i would assume if there was anything left in there ( as minute as it would be ) it would still be present in future extractions.

I am kind of disappointed the whole thing wasn't a success. especially after actually seeing the white stuff emerge in the freezer.

I think after reading other teks, i had the wrong impression that i would end up with the xtals, even if the solvent was evaporated without a freezer.

I've just read through this other thread Endlessness, so i'll be taking those suggestions on board the next time i encounter this problem. Although i still imagine even after turning it upside down, the xtals would still melt with the naphtha they're still soaked in.


After this attempt, i'm still not sure using a larger amount of bark would be a good idea until i get better results with the smaller tester ammount.

back to the drawing board anyway. all a learning curve.
 
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Hi. First post here. Looking for some help on my extraction. :) Any advice would be greatly appreciated.

Using this tek:
1) dissolve 5g of citric acid per 100ml acetone

2) take the shredded/powdered bark and cover it with enough citric acid acetone. Incubate in a warm place, gently agitating every so often. After 2-3 hours, filter off the citric-acid saturated acetone extract and set aside (this solution should have acquired the dark reddish colour of MHRB). Repeat 2 more times.

3) saturate acetone with fumaric acid. Acetone can hold ~20mg/ml fumaric acid if let for a day or so to completely dissolve.

4) Add the fumaric acid-saturated acetone in the citric acid-saturated acetone MHRB extract. One cannot put too much.

5) Set it aside and wait for 2-3 days. One should see a yellowish precipitate on the bottom.

NOTE: In step 2 one is making an acetone extraction and at the same time converting the alkaloids their citrate salt. After addition of the fumaric acid-saturated acetone in step 4, there is an interconversion of alkaloid-citrate to alkaloid-fumarate salt, like:

dmt-citrate + fumaric acid <-> dmt-fumarate + citric acid

citric acid has a pKa of 3.13, while fumaric acid's pka is 3.43. Fumaric acid is a weaker acid and thus in the above reaction one should have most of the dmt as a citrate salt and just a tiny amount as a fumarate salt. dmt-fumarate however is totally insoluble in acetone (while dmt-citrate is perfectly soluble), and it precipitates as soon as it forms. The insolubility of dmt-fumarate acts therefore as a "sink" and given time all of the dmt-citrate will eventually convert to dmt-fumarate and precipitate out.

6) wash the precipitated fumarate salts with acetone, then take them out and let them dry.
Click to expand...

I used 50g powdered MHRB, washed the powder twice using acetone and citric acid solution.
At step four, when mixing the Fumaric acid acetone and dmt-citrate acetone solution, within a few seconds a quite large amount of powder settled to the bottom of the jar. This surprised me because the tek states the dmt fumarate would take several days to precipitate.

I filtered the powder and set it to dry. The powder turned goopy and dark and eventually dried enough and formed a sticky dough. I need help to identify what this material is and what did I do wrong? Is this jungle spice? might it contain dmt?

pictures:
http://img.photobucket.com/albums/v233/Goshikyu/IMG_20110918_170336.jpg (precipitate in the jar)

 
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Hello all,

SWIM has been attempting 69rons d-limonene tek for extraction of cactus alkaloids... like a fool, SWIM decided to use less orange oil than indicated by the tek..... SWIM got impatient and figured hey, less solvents just means more pulls right? well, not with dry teks.....

*

900 ml d-limonene was added to 500gm of cactus that met all other standards of the tek.

when attempting the first pull about 400 ml of solvent was retrieved from the plant material. extracted as indicated and the solvent was recycled. the 2nd pull may not happen. almost no d-limonene is being retrieved from said imaginary jar of cactus.

*

SWIMs question, can the plant material be salvaged after exhausting any further pulls without acquiring more d-limonene (expensive, takes weeks to arrive, etc)?

could for example, SWIM dry out cactus material (does d-limonene evaporate cleanly?) after retrieving as much d-limonene as possible, waiting for the excess solvent and water to evaporate, then use xylene to extract and continue salting with either acetic or hydrochloric acid?

is there any quicker way to fix this (that may not require drying out plant material)?

any incite would be greatly appreciated.
 
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Hello, swim is having a couple of problems with the lazyman tek (he'd be using a more advanced one but he's on a gas stove, and the naphtha...)

I've searched for answers to this problem for my friend, hopefully I'm not just stupid at searching, but I can't find him an answer so I told him I'd post for him.

Anyways, when Swim is stirring his naptha/MRHB suspension back into a mixture, as the suspension unmixes, the naptha and the MHRB never fully separate. So, when swim pours the top layer onto the glass plate to prepare for CFC, as more naptha evaps, he notices that there are small bits of tree bark (he thinks) mixed in with the crystals.

Swim is using 1 lb of MHRB, 375 mL naptha, and he used 17 tbsp of NaOH

How does swim get the small bits of tree back into the solution?
 
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Hello,

This is my first post but I have been a reader for many months on all sorts of forums.
Most of my queries and problems have been answered however I just want to double check.

I just finished super saturating my naptha and it is now in the freezer ( I hope it's cold enough but I doubt it ) Does this really matter if the freezer is not cold enough? There is not much i can do about the temp :(
During the evap stage is it normal for the white crystals to form on the walls of the jar? Have I left it to evap for too long ? Have I ruined it

I used way too much naptha I got my measurements a bit wrong so I evapted about 60%-70% of the original amount.

How long do I need to really keep it in the freezer i've been hearing all sorts of numbers from 6 hours up to 72.

BTW it's in a sellotape sealed jar.

Also it seems to me that after the freezing and filtering the naptha through coffee filters. There could still be some more DMT in the naptha or am I wrong.
Could I not evap and freeze again after filtration? or is this a waste of time for what DMT is left?

Many Thanks :)

TYO

P.S I presuming it's safe to post this because this site is HTTPS. The last thing I need is to get in trouble.
 
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It's supposed to crystallize on the walls so don't worry.

Since you evaporated your solvent 70% chances are all the DMT has precipitated. I wouldn't bother evaporating the naptha to collect anything in there. Just pour it off, dry, and scrape the jar.

And yes, this site is secure. The only thing that is logged is this post, but on the server, that is encrypted to the max. You're fine ;]

Welcome to the DMT-Nexus!
 
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spice does not freeze precipitate out of limonene, as it says in the FAQ. You have to salt it out.

What do you mean with "at the end of the extraction he obtained a lot of white powder" ? What step where you doing before that, please describe your method.

Water will dissolve sodium carbonate and not dissolve dmt freebase. Thats why if you follow BLAB tek and the water conversion you can dissolve dmt fumarate in water, add a bit of sodium carb saturated water and fridge(not freeze) precipitate the dmt out of water
 
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