Problem with viscous stuff after A/B

[rawwrr]

Hello,

I'm new to this board and I want to share SWIM's knowlege about chemistry. SWIM is also active at another board (DF). If someone is curious what's his username is there, please PM me.

Because I'm a new member, I have to post here, so I excuse myself for maybe not posting in the right subforum.


SWIM wanted to extract 100 g Mimosa Hostilis to get some nice, smokable DMT crystalls, but now he has some problems.

SWIM did 3x pulls with dH2O, acidified with HCl, based with NaOH and extracted 3x with xylene, then he washed 2x with Ammonium Hydroxid, followed by another dH2O wash, after that he evaporated with low heat and a fan. This method is mostly the same as Shaggy's Jugle Tek and The DMT Handbook.

As most of the liquid was evaporated he tried to crystallize out the DMT, but nothing appereared, it's just an oily viscous stuff. Even after a whole night blowing with a fan, it's still the same gooey reddish X.

It smells very sweet and disolves in xylene or acetone (tested both).

So what can SWIM do? :/ His ultimate goal is to get nice DMT crystalls.


Have a nice day!


PS: SWIM doesn't has Heptane, just Acetone, Xylene, Toluol, IPA, Ethanol, HCl, NaOH..

 

[rawwrr]

SWIM now thinks this a jungle-alkaloid mix with some xylene left. He is now blowing with a fan, scrapping oily stuff together and spread it over a larger pyrex dish and repeat this till is's dry.

Anyway, he asks himself how he could grow crystalls now. Would it be sufficient to dissolve that dried X into heptane and then do a freeze-precipitation? Maybe he can get naphtha from "lighter fuel" in Germany. To craify: naphtha is "the heptane for poor people"?

Another thing: SWIM read, that when mixing jungle X with naptha two layer will form, is this information also valid for heptane?

 

[gammagore]

You will have a very hard time getting that to crystalise, xylene pulls are always gooey, full range goodness.

Once you have gotten it to dry as much as possible, dissolve it in some warm naptha let it sit for a minute, then you will notice a brown layer at the botton of the glass or whatever you disolve it in, carefully remove the naptha layer and freeze that, this way the naptha pulls just the nn-Dmt.

 

[rawwrr]

You will have a very hard time getting that to crystalise, xylene pulls are always gooey, full range goodness.

Once you have gotten it to dry as much as possible, dissolve it in some warm naptha let it sit for a minute, then you will notice a brown layer at the botton of the glass or whatever you disolve it in, carefully remove the naptha layer and freeze that, this way the naptha pulls just the nn-Dmt.

Thanks for that information, that's what SWIM read before.

Can heptane used in this step instead of naptha?

 

[gammagore]

Sure it can

 

[rawwrr]

Thanks again. Now it's getting drier and drier, but it's harder to spread it over the dish, because it clumpts together.

This extract as it is should also be active, but how to calculate the dose? SWIM want's to start at treshold level, so he thought - if this were n,n-DMT, he would begin with say 5-10 mg.

To use heptane and seperate the two layers it should be complete dry, right?


Sorry for SWIM's beginner questions.. If SWIY is interessted in extracting that jungle X with xylene, he can post a full pictorial.

 

[gammagore]

Does it smell of xylene at all? Id imagine it does, what i do is dissolve it in some pure acetone(i suppose heptane would work too), let evap and dry and if all xylene smell is gone then im good to go. If you want to test what you have after all the xylene smell is gone, then yes 10mg would be a good starting point, and work your way up.

If you do want to separate the nn-dmt from the gooey, it should be as dry as possible. Well it wont get hard, but get it as dry as possible before you add the heptane.

And yes please, we here at the Nexus love pictorials

 

[rawwrr]

Sad news: SWIM didn't found Heptane at his pharmacy and ordering would take some days.. could Zippo lighter fuel be used as subsitute for naptha?

He'll think about the pictoral, maybe it would be better to post it with the next batch, because then he'll have much better results and not that fight with some gooey X.

 

[rawwrr]

Update:

SWIM brought Naphtha and extracted from his mostly dry, but still a bit viscous jungle spice and did a freeze precipitation, at first it seems to work as expected and than he wanted to do another re-x to grow some nice crystalls.

He put his spice in a beaker and the beaker into a cooking pot, filled with ~70° Celsius water. In another beaker he poured some Naphtha and waited, till is was hot enough. Then he pipeted just as much hot Naphtha to disolve all spice. There he realized there were some particels still in solution, which he filtert by transfering the Spice-Naptha with a syringe, which was attached with a cigaret-filter at the needle, into another beaker, to leave all impurities behind.

Then he seeled the beaker and slowly cooled down to room temperature. After a day (he wasn't at home, so no hurry) there was already a really nice white crystall in his jar and he was very happy about it.

Because he wanted to get "perfect" crystalls he then reheated the waterbath to ~50° Celsius, so all the small crystalls will disolve again, while the big one remains, so he should grow even bigger crystalls over time. His plan was doing this "heating, cooling" cycle several times, beginning with hot water bath <-> room temp, room temp <-> refrigerator, refrigerator <-> freezer.

But after the jar was sitting and the nice crystall formed and he reheated the waterbath to ~50° Celsius and letting it cool again to room temp he suddenly saw there is some orange, oily stuff again at the bottom. How did this happen?

 

[gammagore]

Because he wanted to get "perfect" crystalls he then reheated the waterbath to ~50° Celsius, so all the small crystalls will disolve again, while the big one remains, so he should grow even bigger crystalls over time. His plan was doing this "heating, cooling" cycle several times, beginning with hot water bath <-> room temp, room temp <-> refrigerator, refrigerator <-> freezer.

But after the jar was sitting and the nice crystall formed and he reheated the waterbath to ~50° Celsius and letting it cool again to room temp he suddenly saw there is some orange, oily stuff again at the bottom. How did this happen?

So you first managed to get DMT xtals, then you wanted to get them bigger so melted them again in the 2nd hotwater bath, did you add any naptha to this 2nd bath or did you just melt the DMT?

Also you say that you used a cigarete filter, to filter out these "particles", not sure about what them filters are made of, but id be wary of using them. Hopefully the naptha hasnt pulled any impurities during this filtering process.

 

[rawwrr]

Well, SWIM has a jar with Naphtha + solved DMT, which was supersaturated at 60° C, then he sealed the jar and let it cool to room temperature. After a day there were nice white crystalls on the bottom of the jar, but as he read in another thread, it is valuable to heat again a bit, to get smaller x-tals back into the solvent, to let them form bigger ones. He tried this by raising the temperature back to 50° C in a water bath, the jar was still the same with Naphtha + DMT. After cooling down again he saw that some orange stuff formed on the bottom inside the jar, which was not present at his initial cool-down.

At another forum someone else adviced to remove this "dirt" with a syringe, but that's strange, because above the orange there are still the nice white x-tals, so removing would be difficult.

His intention was to follow this procedure with cooling and reheating, till he ends at freezer.

SWIM is just wondering, because the orange wasn't there before and don't know what to do now.

 

[endlessness]

I dont know what the orange is. It may be dmt n-oxide (active and ok), it may be some weird impurity from naphtha or from those filters (not ok), or it may be plant oils (ok but you could remove them).

I think its a bad idea and unnecessary complication to do what you did of heating the naphtha after some of the crystals were already there. Its much simpler to just let the solution cool to room temperature, then alternate between room temperature and fridge every couple of hours, and then the same from the fridge to freezer every couple of hours, and back to fridge and room temp, etc, until eventually going for overnight in the freezer. This is already enough temperature alternation to grow your crystals, heating will increase chances of n-oxide formation and what not (and specially filtering with cigarrete filter is weird idea).

If I were you I would evap all that you have, and recrystalize it with minimum amount of warm naphtha, and into the freezer.

Make sure your naphtha (or solvents in general) evaps clean before using it

 

[rawwrr]

Thank you again. SWIM thinks this was a so called "learning-batch" at all. Next time it'll work with much better results and he will use naphtha from the beginning and no xylene.


Regarding the filtering. As he saw some undissolved particles floating in his solvent, he thought about how to filter them whitout using filter paper, which would soak up way too much solvent (it was only about 10 ml). So he remembered he read that heroin-addicts use cigarette filters to soak it through with a syringe. It turned out this worked very well so get a really clean solvent. (but don't know if any X from filters are dissolved in naphtha now)

After some research: cigarette filters are cellulose acetate with a some triacetin (which acts as glue or something like that).

 

[gammagore]

this triacetin could be dodgy stuff, im no chemist, but id be wary next time about using cigarete-filter's.

I wonder weather any trace amounts of triacetin would have been pulled along?