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First STB extraction - white & yellow crystals Options
 
ChemEng
#1 Posted : 1/26/2009 6:03:22 AM
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image links to larger version.

The vial on the right contains almost pure white snow with a hint of yellow. After reusing the same naphtha and applying some heat for subsequent pulls SWIM obtained the waxier yellow crystals on the left. The crystals were freeze precipitated with a single freezer-countertop-freezer cycle then dried using a furnace vent (hot dry air). SWIM noticed some oily liquid which did not evaporate and may be partly responsible for the yellow color.

SWIM is planning to do a recrystallization by mixing all the spice together with just enough clean, heated naphtha to dissolve everything, then separating the naphtha layer from any impurity layer and freeze-cycling to form thicker crystals. Will the recrystallization help to remove the yellow impurities, or will it just spread them to all the crystals? Is it possible that SWIM applied too much heat & air, forming some N-Oxide which would be inseparable from pure N,N?
 

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shoe
#2 Posted : 1/28/2009 8:48:57 AM

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OH MY GOD!!!

lol, well done Smile

that is very well done, not just for a first time, but even just in general!
shoe

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shoe
#3 Posted : 1/28/2009 8:51:21 AM

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just out of interest, what was the yeild there and how much mimosa (or otherwise) did you extract from?
shoe

ॐ भूर्भुव: स्व: तत्सवितुर्वरेण्यं । भर्गो देवस्य धीमहि, धीयो यो न: प्रचोदयात्
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ChemEng
#4 Posted : 2/1/2009 9:28:57 AM
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SWIM's yield was in the range of 0.9 - 1%.

from 1300 g MHRB in three separate 430 g batches, approx 12 g of spice Cool I believe a further 2-3 g would have been possible using additional pulls and/or a xylene pull. considering this is for personal use i think SWIM went slightly overboard..

i would be happy to answer any questions about SWIM's technique or materials in case anyone is trying their own extraction.
 
sentient
#5 Posted : 2/1/2009 10:10:18 AM

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@ChemEng-

Wow very nice results. My friend is doing this for his first time, would you be so kind as to provide your method of extraction.? SWIM will be using MHRB for the source.

Thank you
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ChemEng
#6 Posted : 2/1/2009 4:55:10 PM
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SWIM used the basic STB method. 430 g powdered bark, 3000 mL water and 200 g lye were added to a plastic gallon container. (In the future SWIM will probably use slightly less bark for the same amount of lye/water, maybe 350 g) The container was shaken vigorously every half hour or so for a few hours and allowed to stand overnight. 300 mL naphtha (Ronsonol) was placed in a jar, swirled in a hot water bath and added to the container. (You may want to use slightly less naphtha, something like 200 mL) The container was gently rolled every few minutes for about 1 hour, then allowed to settle out into layers. The layers were separated with a turkey baster (modified to reduce the diameter of the nozzle). (Tip: ensure NO basified bark mix droplets get pulled with the naphtha - leave a layer of naphtha at the end if necessary). The pulls went into glass mugs which were covered with tinfoil/elastic band and placed in the freezer at its coldest setting. After 12-24 hours the cold naphtha was poured off quickly & carefully (SWIM did not bother with coffee filters) and the crystals air-dried (without fan or heat to slow formation of N-Oxide - best method is to raise the bottom of the jar so that excess naphtha trapped in the crystals can drip out slowly) while the naphtha went back into the container for the next pull. For the last pull (5th) SWIM heated the entire container in a warm water bath for 1 hour (no hotter than 40 C or 104 F) which yielded the waxier yellow crystals. A recrystallization was used to purify the final product which is stored in airtight vials in a paper bag in the refrigerator to protect it from moisture, light & heat.
 
xx13w7xx
#7 Posted : 2/1/2009 8:18:11 PM

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I would recrystalize both of them seperatly..
No need to even risk contaminating the pure spice, you know?
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sentient
#8 Posted : 2/2/2009 4:54:43 AM

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Great, thanks for the quick reply. SWIM has been reading a lot of teks, trying to get all the pointers, and learn from the experienced. SWIM is just about ready to get some MHRB.

It seems for the most part people are not too concerned about de-fatting when using MHRB. In this tek it says defatting will help with yields. Here it is if anyone is interested. SWIM will be using this tek unless someone can provide a better one.

http://www.erowid.org/ch..._extraction_guide1.shtml
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ChemEng
#9 Posted : 2/2/2009 5:01:14 AM
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With MHRB it's not necessary to defat especially if you do a recrystallization. The fat/oil content in MHRB is very low. That tek looks overly complicated and the yields will likely be lower due to the extra steps and filtration. STB has some of the best yields out there especially if you follow the naphtha pulls with a xylene pull.
 
shoe
#10 Posted : 2/2/2009 6:25:16 AM

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I just wanted to say that SWIM doesn't defat; and he also evaporates quickly with an electric fan heater, whether or not this produces more n-oxide isn't certain but he feels that it doesnt affect the quality of the trip significantly whereas it does allow the product to be utilized alot quicker than usual. (30 mins - 1 hour) instead of 4 - 5 hours with a fan but no heat.
shoe

ॐ भूर्भुव: स्व: तत्सवितुर्वरेण्यं । भर्गो देवस्य धीमहि, धीयो यो न: प्रचोदयात्
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acolon_5
#11 Posted : 2/2/2009 2:26:35 PM

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xx13w7xx wrote:
I would recrystalize both of them seperatly..
No need to even risk contaminating the pure spice, you know?


I was just going to write this.

Your cleaner batch will recrystalize into some amazing glass shards.

The yellow may need more than one...but you may want to keep a bit of the yellow around as is. Some prefer it.
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I am certifiably insane, as such all posts written by me should be regarded as utter nonsense or attempts to get attention.

I don't know SWIM and personally don't trust him at all. If SWIM is posting, most likely I will not respond...as I said, I don't trust the guy. YOU I trust, but never SWIM.
 
sentient
#12 Posted : 2/2/2009 11:59:42 PM

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ChemEng wrote:
With MHRB it's not necessary to defat especially if you do a recrystallization. The fat/oil content in MHRB is very low. That tek looks overly complicated and the yields will likely be lower due to the extra steps and filtration. STB has some of the best yields out there especially if you follow the naphtha pulls with a xylene pull.



Thank you again for your opinion, I agree there seems to be a lot of steps in that tek. I am pretty new to these forums, and I apologize for the noobness. Could you please provide me the link to the STB method you used? Thanks for all your help.
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ChemEng
#13 Posted : 2/3/2009 12:12:37 AM
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I used an amalgamation of several teks, adapting the techniques to the equipment I had on hand and modifying some of the steps that are unnecessary. My above post explains pretty much all there is to the technique. I would be happy to answer any specific questions you may have.

These are some of the sources I used:

Alien Tek
http://www.shroomery.org...php/Cat/0/Number/8119027

Lazyman's Tek
http://www.entheogen.com...um/showthread.php?t=9217

Noman's Tek
http://www.dmt-nexus.me/...s_dmt_extraction_tek.pdf


 
sentient
#14 Posted : 2/3/2009 12:23:09 AM

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ChemEng wrote:
I used an amalgamation of several teks, adapting the techniques to the equipment I had on hand and modifying some of the steps that are unnecessary. My above post explains pretty much all there is to the technique. I would be happy to answer any specific questions you may have.

These are some of the sources I used:

Alien Tek
http://www.shroomery.org...php/Cat/0/Number/8119027

Lazyman's Tek
http://www.entheogen.com...um/showthread.php?t=9217

Noman's Tek
http://www.dmt-nexus.me/...s_dmt_extraction_tek.pdf





You are a gentlemen. I will be back in about 1 week when SWIM gets his Supplies. I will read those teks you provided in the mean time. Hope to coordinate with you when SWIM is geared up. Fuck, the excitement is getting the best him. XD
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sentient
#15 Posted : 2/3/2009 1:22:16 AM

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Ha, Im back again Just to clarify, So no need buy HCL or something cause its only required for the de-fatting?

Here is my understanding of the proceedure you(ChemEng) listed which I like a lot better than the one I was planning to use. please let me know if you see something that needs revision:

1. Basify the water to ph-12
2. Soak the MHRB with the basic water, stir, role container, avoid creating emulsion . Let sit 24h.
3. Warm Naptha in water bath. then add to container stir/mix well. Then allow to seperate.
4. Syphon naptha layer and deposit into glass dish.
5. Set freezer on max and place glass dish in 12 hours.
6. Someone please tell me the best way to collect the crystals from the naptha without spilling, or have a coffee filter possibly rob some spice from the naptha.
7. Save naptha and repeat from step 3.


Basically just re-wrote what you already said, but I just want to be 100%
XD

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ChemEng
#16 Posted : 2/3/2009 1:51:55 AM
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The naphta does not convert it to a salt. The DMT freebase (the product of this process, and the one most suitable for vaporization) can be converted to DMT fumarate salt (the water-soluble variety, best for any other method of ingestion) using a process which involves zinc powder. I have no experience with this however.

1. AFAIK the PH should be close to 14 (13.7 or something).

2. There is no need to worry about creating an emulsion prior to adding the naphtha. Mix the bark/lye/water mix as vigorously as you like. It's only after you add the naphtha that you have to worry about emulsions.

5. I would use 18-24 hours in the freezer if you aren't pressed for time, to ensure all the dmt is formed into crystals.

6. Every time I've done it, the crystals have stuck to the sides of the glass so that I could pour the naphtha out without any of the crystals going with it. I haven't seen the need for filters of any kind. It's important to pour out the naphtha very soon after taking it out of the freezer to ensure the crystals don't dissolve again into the naphtha as it warms up. Even if a small amount of DMT goes out with the naphtha, you'll be able to collect it later when you re-use the naphtha for another pull.

Once the majority of the naphtha is out, I prop up the bottom of the glass so that the excess naphtha that's trapped between the crystals can drip out slowly. Once the crystals are dry (no more smell of naphtha - just the plasticky smell of DMT) scrape them off the sides of the glass using your tool of choice (knife, spoon or razor) and store them in an airtight glass container away from light & heat in the refrigerator.

You may notice the edges of the white crystals turning yellow during the drying process. This is normal and indicates formation of small amounts of DMT N-Oxide.


 
ChemEng
#17 Posted : 2/3/2009 1:58:54 AM
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One more thing, be careful when pouring naphtha because it tends to run down the side of whatever container you're pouring it out of! It's best to use a tall glass or jar which is less than half full of naphtha so that it's moving in a fast, narrow stream by the time it reaches the rim of the glass. A funnel also comes in handy.

You are correct, there's no need to buy HCL if you omit the defatting step.
 
sentient
#18 Posted : 2/3/2009 2:06:06 AM

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Lol.

You replied as I was editing my previous post, but have still answered all my questions. You have been of tremendous help, and I appreciate your speedy insightful replies. I read somewhere that if the ph is higher than 12 then it alters the molecular stucture of dmt and can result in a lower yield. I will still follow your instuction however unless you tell me otherwise. You seem to have a good handle on chemistry, and your results look very impressive.
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modsquad09
#19 Posted : 2/3/2009 2:06:20 AM

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acolon_5 wrote:
xx13w7xx wrote:
I would recrystalize both of them seperatly..
No need to even risk contaminating the pure spice, you know?


I was just going to write this.

Your cleaner batch will recrystalize into some amazing glass shards.

The yellow may need more than one...but you may want to keep a bit of the yellow around as is. Some prefer it.


thats all ive ever smoked was the yellow stuff..

what would you say is the difference acolon?
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ChemEng
#20 Posted : 2/3/2009 2:22:51 AM
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sentient wrote:
I read somewhere that if the ph is higher than 12 then it alters the molecular stucture of dmt and can result in a lower yield.


All the teks I linked to mention a required pH of 13.5 or higher. I believe this is to break down the naturally-occurring DMT fumarate salt into the freebase form, which is the one that readily migrates into the naphtha.

I'm curious which method you plan to use to vaporize the final product? I heartily recommend the VaporGenie (with 4-5 extra 5/8 inch screens of the finest mesh available to keep the molten dmt from dripping through). http://www.vaporgenie.com . It's much more pleasant and effective than messing about with a light bulb or test tube vaporizer.
 
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