• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Problem with Freeze Precipitation.

Migrated topic.
If she can get pure naphtha/hexane/heptane, yes definitely recrystallize. Redissolve in minimal amount of hot solvent and freeze. Use just as much hot solvent as can dissolve most of the oil after some mixing, but leaving a darker goo behind. Then freeze precip.

If those solvents are not possible, another option would be to just infuse some herb with the oil and smoke that instead (weigh the herbs before and after infusing to know total weight of alkaloids).

Yet another option would be to redissolve in a solvent, even if its this same one, and salt it out with FASA or FASW or maybe FASI. Then do the water crystalization with sodium carb as described here, and she should get her crystals
 
Quite a few times swim ended up with red-brown goo with no sign of crystals. This has happened regularly back in her STB days and every time she tried Panoramix's pseudo-A/B tek.

Trying both re-x and mini A/B she has found that a mini A/B is much more reliable procedure. Actually she has read in a chem book that if a substance is too dirty re-x is not an efficient way to clean it. So, if there is any spice there a mini A/B should do the trick.
 
Ok, this has got to be the most long winded extraction from Hell, going wrong in almost every step!

I got informed by my friend that what she did was this:

1)Scraped the dish where she evaporated all the pulls together, after she put it in the freezer. This afforded a sizeable amount of "honey dark brown" goo with no signs of crystals.
2)Added 10 ml of hot hexane,and put the whole thing in hot waterbath stirring continuously.
3) The goo would not dissolve, it liquified but the hexane stayed on top, acquiring a yellow milky color.
4)The whole thing was put into freezer for the procedure to continue another day. The bottom part (goo) froze solid, the top part of the goo became white and in the hexane layer it seems that something white opague is falling out of solution but as very fine particles.

I wonder if she can reheat and "extract" whatever can be picked up from the goo using hexane washes on it...

The first two pictures is before freezer, the next two is after freezer. It seems that the hexane picks up something from the oily mess that is at the bottom. I really wonder why the whole procedure proved to be unexpectedly hard...
 

Attachments

  • Profreezer1.JPG
    Profreezer1.JPG
    32.5 KB · Views: 1
  • profreezer2.JPG
    profreezer2.JPG
    35.6 KB · Views: 1
  • afterfreezer1.JPG
    afterfreezer1.JPG
    42.9 KB · Views: 1
  • afterfreezer2.JPG
    afterfreezer2.JPG
    28 KB · Views: 1
I dont think she should have put the whole thing in the freezer, only the milky heptane. That was kinda weird decision :D

Its probably not enough heptane and thats why plenty of other stuff didnt dissolve. Also, impurities indeed should not be dissolved, its better to use just enough heptane to dissolve most of the product but leaving a goo behind.

What I would probably do is an A/B on the whole thing. Let it warm up to room temperature, put in a container, do 3x vinegar pulls, throw solvent away, re-basify vinegar layer, re-extract (small pulls) and into the freezer.
 
A Small update : My friend informed me that she washed the "red oil" 5-6 times with hot hexane, and put it in the freezer (the hot hexane pulls). She told me that it seems to go opaque when she blows on it, surely it seems as if she cleaned it up a bit so she is waiting for the freezer results. Nothing was thrown away though...

Now, on a related note the bark seems to be fine and it seems to have contained DMT. Let me tell you that "Seems" is rather an understatement! She called me over, because she wanted me to take care of her and supervise her : she was planning on smoking some of the red oil (pre-hexane treatment) , specifically a miniscule quantity that was left on a razor after she had scraped the pan so as to transfer it in the small jar pictured in a previous post.It was a miniscule amount, it was what stuck on the razor and could not transfer in the jar due to the sheer minute amount of it. Well, i gave her the talk , not to be dissapointed if it didnt work, she should expect visual disturbances at best since the quantity was small and since certainly it was not pure.I also told her not to panic if it proves to be a little stronger than that. Well, she took 2 puffs of it from some tobacco using a bubbler and...she was blown away! My jaw dropped because she seemed totally engulfed in it, she was obviously under the influence! Her jaw dropped too, i couldnt tell if she was terrified or ecstatic but i remained a spectator so as not to interfere.Finally when she exclaimed "Marvelous!","Extraordinary" and "It cant be!" i was sure she was ok. She also saw "entities", a "light being" emanating "goodness" as she discribed and a playful "chimpanzee like entity".

The good/weird part? That amount was enough to give her 3, almost 4 sub-breakthrough experiences, i mean in the jar its about 40-50 times that amount! The amount was miniscule and...its almost ridiculous how potent it was.Ridiculous to the point i thought she could have been pulling my leg,if i hadnt seen her reaction myself i would seriously doubt the potency from such an amount! A happy grin stuck in my face because after all it seems that she had not failed the extraction and quite literally she got more than she bargained for, so im happy for her! On her behalf, i want to thank you and of course will continue to update if she sees crystals in the freezer. Yup, the bark was more than good!

On a related note : The red oil/goo is rather difficult to get off the hands and smells very very very pleasantly floral!! A very peculiar smell, like no other!
 
ive had the same experience with the orange/amber fraction you get from a stb with petro solvents. it seems many times stronger. and more powerful

but ive come to believe that it has more to do with the difference in density of dmt oil and crystal. i store my spice 100mg/.5ml glass vial. when using yellow or white spice i have to pack it in. when using pure amber oil with just enough nn-dmt added to cause hardening. its like 5% to make the oil solidify. this cake/shard can be packed 300-500mg/.5ml vial.

so when i give someone the experience, if i give them 50mg vaped. out of the 20ish people i have launched, about 3/4ths prefer the orange/more oily trip. this is before my having influenced their mind by telling them the difference. i just ask which they would like. then the other, then explain it.

i gave an oldhead i know some of the 95/5 amber product and he said it was the most spiritual feeling tryptamine he had felt. i tend to agree. the oil, in my bias experience, seems more body, inward, dark, powerful, and arcane in nature. as if instead of being shot down a railgun into hyperspace, you cave inward into your mind and beneath it into a wormhole. ive seen amazing visions, yet much less open eye distortion than with white spice. ive gone to the beautiful infinite crystaline machine via 95/5, but ive also had amazing visions. like.. vape it.. world darkens, gains depth, and fades. impending doom..? no, pure euphoria. then suddenly a surge of dysphoria being experienced while still feeling full euphoria. then nothing. for how long?.. now i am nothing. a dreamstate. and here i see things in real world quality. full vision/mind imagination. massive influence over what i see. a drug induced lucid dream. 10min later it fades to a twisted warm tryptamine. if i lay still, and delve into my mind, i can remain here for 30-70min. if i awake myself or my environment does, it vanishes quickly. my white/light yellowish clear spice causes me a much more visual fractal infinite depth scenes. bright. colored. typical hyperspace/alien feeling =]
 
Not wanting to open another thread, but with the danger of this question being overlooked, i decided to post it here:

I see on the solubility list (wiki) that freebase DMT is listed as "very soluble" in ethanol compared to "soluble" in hexane. Could one use ethanol to clean DMT (pick it up to seperate it from oils), or it would pick up oils?
 
Back
Top Bottom