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First few STB extractions done..My Detailed Comments...Now what? What went wrong? Options
 
HotTuna
#1 Posted : 7/30/2010 10:59:19 PM
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Hello all. Been lurking for a while before signing up and SWIM took a crack at an STB extraction. Did lots of reading up on different TEKs, materials, labware, Recrystallization, and whatnot so SWIM felt somewhat well read and up to date on techniques. Have read some advanced methods and TEKs but felt to go simple due to popularity, ease, and effectiveness.

Abstract:
SWIM attempted this OZTek 15 Min STB heptane TEK: https://dmt-nexus.me/forum/default.aspx?g=posts&m=153156 and http://www.shroomery.org/forums/showflat.php/Cat/0/Number/12738710
SWIM followed directions pretty closely...And yields were VERY LOW from 3 pulls. Off the bat, SWIM thinks the root was to blame.

First time half-weight Tek. Second time full weight tek.


SWIM's overall Observations:
1. Mixing NaOH solution got in excess of 180­°F
2. Nalgene Labware can handle the heat without issues.
3. MHRB Solution sticks to inside walls of nalgene containers making clarity and decanting. Is this Normal? Also did the same in glass container.
4. Clarity of Nalgene O.K.. Very difficult to see line between heptane and MHRB solution.
4a.Seperation of heptane from solution very difficult to do with pipette and also Sep Funnel. Inside walls of sep funnel extremely dirty with MHRB. Making Sep Funnel useless due to contamination.
4b.Something like a graduated cylinder with a smaller diameter seems like it would be easier to pull off.
5. Heptane was very yellow upon seperation. Lemon-lime gatorade
6. Freeze precip(FP) worked, but yeilds were very low and waxy yellowish. Also lots od yellow oily matter. Some little white nodules but all mixed up for re-X
7. Re-X process pretty straight forward. Small initial product makes it difficult overall. Oily yellow matter settled to bottom, Hazy, less yellow solution in pipette when pulling saturated solution from water bath. Hazy was a good sign. Slowly cool to room temp, then room temp for a few hours then FP and strain heptane. Yields were unusable and still yellowish waxy. Using Shot glass method
8. The most that ever came out from a pull was about a pea-sized quantity of light yellow waxy matter.
9. What's the best FP container?
10. DMT seems to be soluble in room temp heptane.


SWIM's expectations/reservations/outcome:
1.MHRB solution wouldn't stick to sides of labware/containers. Especially sep funnel. Why?
2.Haven't found use for filtration funnel.
3.Went in with high confidence. Now, total bummer.


Questions:
1. Bad MHRB?
2. Why the clumpyness of MHRB solution? Maybe need more NaOH solution to MHRB ratio? More or less concentrated(higher/lower pH) NaOH solution?
3. Improper TEK/technique?
4. Does each pull have it's own FP or is all of the solvent FP'd at once in one container? SWIM did separate.
5. What effect does temperature of the MHRB solution have on the extraction process? Aside from heating the heptane to allow greater solubility.


Any other comments? input? questions for me?

Thanks for reading and I'm looking forward to an engaging discussion on these issues.

 

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Gir
#2 Posted : 7/30/2010 11:52:27 PM

Gir

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15 minutes = impatience

Take 2 hours. 1 hour for it to completely basify, and 2 half hour pulls, rolling gently constantly.

Youll get the desired results. I dont see why people are posting these "fast way to get it" teks.. Its not like it takes forever to get product ANYWAYS.

-gir
Lets go extract something together Smile

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ragabr
#3 Posted : 7/31/2010 12:16:24 AM

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^^ what Gir said. Also, DMT has a lower solubility in heptane than in other solvents, so it will need a longer soak than naptha or d-limo.
PK Dick is to LSD as HP Lovecraft is to Mushrooms
 
HotTuna
#4 Posted : 7/31/2010 4:26:33 PM
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Thanks. SWIM has patience.

What about the heat aspect? After 2 hours, the solution would be at room temp. Also, are the proportions still good(based on links provided in first post)? i.e. Mhrb solution to solvent ratio and mhrb to NaOH solution ratio?

What about the clumpyness/sticking to inside of containers?
 
ragabr
#5 Posted : 7/31/2010 5:57:42 PM

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The ratios should work fine, and the color (jet black) will let you know. To get the heptane hot enough, boil a pot of water and put a jar with your heptane into it after turning off the heat. Once the heptane starts bubbling, then transfer to the solution and swirl (or shake, according to the tek).

Clumps and sticking seemed pretty normal in SWIM's experiences with STB.
PK Dick is to LSD as HP Lovecraft is to Mushrooms
 
HotTuna
#6 Posted : 8/1/2010 5:48:58 PM
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Thanks. SWIM did some experimentation with ratios on a 50g MHRB extraction.Minimal clumpyness. First pull(non white spice) 830mg. Swim's 2nd pull is separating then FP.
 
zeekborg
#7 Posted : 8/1/2010 8:15:40 PM

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In regards to the MHRB sticking to your containers, I did a different tek then you (just an acid/base with lye and vinegar) and after the acid wash I decanted the liquid into a different jar before adding the base. This got rid of 99% of the RBP floating around and made the rest of the tek really easy to see and do. If you don't wanna do the acid wash I'm sure once you let the basify solution settle you could decant the liquid off and go from there. Could make it alot easier. Also time is your friend here. I found that I had to let the basified liquid sit for at least 2 hours before I got anything and the longer the better. Try a day. When you go to add your solvent a good way to heat it is add a bit more lye mix around till it's thoroughly heated then pour in the solvent. I shook the hell outta mine didn't care if an emulsion formed because I wanted to let it sit for a long while anyways. When it finally seperated (maybe an hour or so later) I extracted the solvent and put it in a ceramic container for freeze precip.

As for the oily residue I got alot of that in mine and from what I understand its DMT oxides, and although I havent broken through yet (close tho Cool ) I have heard that the oxiedes are more visual (although I haven't tried pure dmt) I can definitely vouch it's very visual

Good luck hope I helped
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HotTuna
#8 Posted : 8/3/2010 3:10:57 PM
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zeekborg wrote:
In regards to the MHRB sticking to your containers, I did a different tek then you (just an acid/base with lye and vinegar) and after the acid wash I decanted the liquid into a different jar before adding the base. This got rid of 99% of the RBP floating around and made the rest of the tek really easy to see and do. If you don't wanna do the acid wash I'm sure once you let the basify solution settle you could decant the liquid off and go from there. Could make it alot easier. Also time is your friend here. I found that I had to let the basified liquid sit for at least 2 hours before I got anything and the longer the better. Try a day. When you go to add your solvent a good way to heat it is add a bit more lye mix around till it's thoroughly heated then pour in the solvent. I shook the hell outta mine didn't care if an emulsion formed because I wanted to let it sit for a long while anyways. When it finally seperated (maybe an hour or so later) I extracted the solvent and put it in a ceramic container for freeze precip.

As for the oily residue I got alot of that in mine and from what I understand its DMT oxides, and although I havent broken through yet (close tho Cool ) I have heard that the oxiedes are more visual (although I haven't tried pure dmt) I can definitely vouch it's very visual

Good luck hope I helped


SWIM fixed the clumpyness by upping the NaOH solution PRB ratio. Nothing sticks to the walls. Especially after adding the solvent.

The only part that is bothersome is that the solvent also absorbs some unwanted stuff (oils?). The solvent is very yellow. Wondering if there's an optimal time extraction time and temperature to minimize transfer of unwanted compounds. Or is there another solvent which will only pull the nasty compounds from the DMT solution?

 
RigelL
#9 Posted : 8/3/2010 6:00:00 PM

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I use naphta for solvent and with me it always gets yellowish, no problem dough, cause tha spice is always snow white Pleased in the first two pulls at least then in the other 2 pulls it gets yellow. Regardless of it´s color it´s still spice, and imo i just luv the yellow spice =)
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