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Acetone/citric/fumaric tek Options
 
trydzyk
#1 Posted : 10/14/2008 9:18:17 AM
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Hello,

I found this interesting tek, while looking for alternate extraction solvent ("naphta" is unavailable in my country). This is NOT standard A/B tek or STB tek, this is something new, though slow. I am planning to try it next, as it seems I've already wasted 200 mg of MHRB with no yields...

Original publication: http://www.drugs-forum.c...m/showthread.php?t=68002

The tek:

1) dissolve 5g of citric acid per 100ml acetone

2) take the shredded/powdered bark and cover it with enough citric-acid saturated 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 <-> dmt-fumarate

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.

7) dissolve the alkaloid-fumarate salts in 5ml of tap water, then and then add saturated sodium carbonate to make the solution basic. The alkaloids will be freebased and the solution will become milky. In 3 days they will precipitate out forming nice needle-like crystal in the basic solution. At this stage, one can filter the solution (nasty procedure since the crystals tend to be sticky and waxy) and retrieve any left alkaloids by dissolving them in acetone.

Cool Let the crystals dry, wash them with acetone (it removes any traces of sodium corbonate which is totally insoluble in acetone), evaporate the acetone and enjoy the product.

For the FOAF of SWIM 30mg were for a good STRONG experience.

Control: If no fumaric-acid saturated acetone is added in the citric-acid saturated acetone extract (step 4) NO precipitates are seen after 3-4 days. This suggests that the precipitates are the fumarate salt of "some kind" of alkaloid.

Considerations:

1) In a pilot experiment of SWIM's FOAF just acetone was ued for the initial MHRB extraction. Addition of fumaric acid saturated acetone did not produce any precipitates immediately and on the other hand this silly guy did not wait for few days to see if anything precipitates.

2) Step 7 can be tricky. Sane humans would most likely go for an already tested A/B extraction using small quantities of a NP solvent.

3) this method definitely takes ages; it relies on the acetone insolubility of the alkaloids' fumarate salts. The rate limiting step is the conversion of alkaloid-citrate to alkaloid-fumarate. This problem could be overcome IF one was using an acid weaker than fumaric acid. This acid must be available in relatively anhydrous form (like the case of citrc and fumaric acids) and must be dissolvable in acetone. A good candidate could be glacial acetic acid (=100% acetic acid) since it has a pKa of 4.75 and is therefore weaker than fumaric acid. But not everybody can get glacial acetic acid easily (as opposed to teh other chemicals used in this method).....
 

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Infundibulum
#2 Posted : 10/14/2008 9:59:38 AM

Kalt und Heiß, Schwarz und Rot, Kürper und Geist, Liebe und Chaos

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Hi,

Do not try it since it is still an experimental technique. Or if one really attempts to try it he should start playing around with it by extracting small doses of MHRB. If a method is not widely used then it is not good enough.

SWIM finds this method a bit hectic but doable. He would not use it as his standard method for future extractions though. The main reason for publishing such a document is simply because they demonstrate other ways to extract spice as well as because they may stimulate someone to propose improvements over the current technique.

One is definitely better off using A/B or STB, naphtha should bot be a big problem to find! How about white spirit, turpentine substitute, Coleman's fuel, zippo lighter fuel etc etc?


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Jorkest
#3 Posted : 10/14/2008 3:03:49 PM

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Moderator | Skills: Extraction Troubleshooting, (S)elf ProgrammingChemical expert | Skills: Extraction Troubleshooting, (S)elf Programming

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first time swim did an extraction...all he could get was odorless charcoal lighter fluid...kingsford i think..anyway...wouldnt use it again...just because...but it DID work...
it's a sound
 
amor_fati
#4 Posted : 10/14/2008 4:10:38 PM

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trydzyk
#5 Posted : 10/17/2008 9:36:11 AM
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Infundibulum wrote:
Hi,
One is definitely better off using A/B or STB, naphtha should bot be a big problem to find! How about white spirit, turpentine substitute, Coleman's fuel, zippo lighter fuel etc etc?


Is white spirit OK to use? I've seen it available in stores here. So's turpentine. Currently I am trying with coleman...
 
Infundibulum
#6 Posted : 10/17/2008 4:21:33 PM

Kalt und Heiß, Schwarz und Rot, Kürper und Geist, Liebe und Chaos

ModeratorChemical expert

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People report it to be OK. SWIM initially had some bad luck using white spirit in the beginning (lack of experience? poor bark?) but later experiments were successful.

Purified spice is soluble in white spirit and white spirit floats on top of the water, so it should be absolutely fine when used for A/B or STB. It does take ages to evaporate though (contains hydrocarbons on the C7-C12 range), so freeze precipitation after pulling with hot white spirit are keys to good yields here.

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
 
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