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Square crystals?

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Swamp_Donkey

Swamp_Donkey

Rising Star
Hey all,
Ok so, im wondering if this is actually the goods or not?
The crystals that formed on the first series of pulls were needle/swordshaped snowball like clusters (sorry no pics). Done via freeze precip.
I decided to see how much more I could pull from the base soup into a different dish(apparently quite a bit considering I thought it was tapped out. The pulls (naphtha) were progressivly becoming more yellow as I went. And instead of a freeze precip I opted for a slow evap thinking I would do a mini AB at the end.

Notes on second series of pulls:
- Obtusi bark, shredded.
- room temp diggers shellite
- 4 x 50ml approx pulls
- A/B extraction used (vinegar/NaOH) with NaCl before basifying
- stainless steel collection/evap dish
- smells strongly of the goods, even more so than the first series of pulls

Has anyone had crystals like this before from a slow roomtemp evap?
Any input appreciated
Thanks yall :D
 

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I never had that because everything melts to goo here up the farNQ. Thanks for the eye candy though. :thumb_up:

Did you heat your soup or shellite at all?
 
The first set of pulls were done in a 55 celcius waterbath. And yeilded little snowball clusters with a small ammount of clear to ever so slightly yellow oil surrounding the clusters.
But the above (pictured) was all done at room temp and left to evap fully.
Im wondering if the different method, evap vs precip could from such different cryastals.
Also salt and NaOH have a similar cyrstal formation, but thats a fair whack of NaCl or NaOH to come through with the np I would think. And no base soup came through with it. The NP fraction was ran through filter paper.
 
Try taking those crystals and oil in the picture and recrystallising from shellite. If they refuse to dissolve, then there is a fair chance they are an inorganic salt, namely sodium chloride or sodium acetate. Try the experiment, add shellite, heat and stir for a while, filter while hot, place filtrate in freezer. Solids in filter paper are inorganic salts, while precipitated solids/oil in the freezer will be dmt and/or nmt. Hope that makes sense.

An easier option is to just add xylene, stir at room temp and filter. Once again, inorganic salts will be in the filter paper.

As for the appearance of the crystals in the picture, if they are not an inorganic salt, I would be surprised.
 
Alrighty,
Everything dissolved..... except for a lil bit of sticky oily crud stuck to the dish.
The crystals dissolved first and quite quickly, then the oily goo. There was nothing in the filter paper besides a faint yellow stain.

Any more thoughts? :?

It is in the freezer now :)
 
Did you dissolve in shellite or xylene?
If using shellite, and you got a crystal clear solution after filtering and you have placed that in the freezer, the next step is to wait 48h. See if you get the typical dmt snowballs.
Looks like I was was wrong. If it dissolved so readily, its likely an organic compound.
Let us know how you go.

After all this, if there is still doubt, you should run this substance through another acid/base extraction to ensure it's an alkaloid.
Interested to hear how you go.
 
I used shellite (diggers)
It was clear and instantly clouded when air ripples the surface.
By clear I mean it was yellow tinged but not cloudy or anything (untill air is blown onto it)
 
Looks good. Mystery solved.
Looks like the big squares were dmt. They may have formed that way due to slow crystallisation during slow evaporation.
Do you mind me asking what your yield was from the obtuse bark?
 
Dicko said:
Yeah man it was 0.6% from 100g :) expected yield was between 0.5 and 0.7 so pretty much bang on. :)
Click to expand...
have you tried more pulls? there may be more left.

I used to do 4-5 pulls until I went up to 8 just out of curiosity and found out that I was leaving ~50% of the spice in a base soup. I got 1.83% instead of usual 0.8%-1%.

Also, try pulling with toluene/xylene after finishing naphtha pulls. you'll get even more.
 
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