neat transparent goo

[Pokey]

To really get a handle on this you must read page 2 of the "idea for obtaining freebase" thread. I made a new topic because that project has changed into a very different chemical experiment (also hoping to attract more blue flask folk that may have gotten bored with the other thread....).

The summary is: I now have a 1000ml container with an alkaloid saturated solution that is ph 11.9. That ph was achieved using lye. It also may contain sodium carbonate, although it seems that most, if not all of the sodium carbonate crashed out of the solution in a previous step of this process when anhydrous IPA was added. When the lye was added to the solution, the ph jumped from 9.6 to 11.9 and the color changed from white and opaque (just like milk), to yellow/orange tinted and transparent.

I have added, mixed, and seperated 100ml of heptane two times hoping to pull the alkaloids from the solution. The heptane is in the process of evaporating and appears to be yielding crystals, how much I don't know yet (seems like it may be quite a bit:d ).

When adding the second 100ml of heptane, I noticed a layer on the bottom of the container of clear, jelly-like material. I shook the container vigorously to see if it would dissolve. It didn't really dissolve, but it did get pretty evenly distrbuted in the solution. I would describe it as being "suspended" or "in suspension" for lack of a better term. The viscosity of the solution changed radically; it got very thick.

This mystery goo seperates and falls to the bottom of the container when left undisturbed for a little while except for some that sticks to the sides- looks almost like crystals, but it isn't. I decanted the solution and nw have a container with about an inch (maybe 100ml) of the mystery goo at the bottom and a little bit stuck to the sides.

Any idea what it is or how I can figure out what it is?


Pokey the Curious

 

[Pokey]

Well I just checked on my container of mystery stuff. The stuff stuck to the sides is drying out and it IS crystals of something. They are small and completely clear. There is lots of the stuff at the bottom that can't dry as I just decanted the liquid from the top by pouring it off into another container which left quite a bit of liquid.

I guess I'll filter the stuff and let it dry. I'm dying to know what it is. Anyone have a theory or a way for a regular person to determine what it is?

It "crashed" out of the soultion on its own, looked and felt gelatinous before drying but seems to actually be a solid crystal of something when dry. The sodium carbonate added previously was white powder and I believe it is not part of the solution anymore (not sure though).

I will filter and dry it now, and post any further developments in this interesting (to me, at least!) experiment.

Pokey

Edit: Curiouser and curiouser....
Got impatient and spread the crystal stuff out on a pyrex pie dish and stuck it in the food dehydrator. When heated it turns into a liquid. Not much help with drying the stuff if all turns to liquid...
Allowing it to cool to room temperture again to see what that does.

 

[Pokey]

Well I feel like I'm talking to myself here as everyone is so focused on the BBB fiasco, but I'll document my experiments for posterity if nothing else.

After returning to room temperature the mystery stuff re-crystalized in to much bigger, totally clear crystals.

When I put it in the food dehydrator (this comparison will only help those who have real winter) it looked EXACTLY like slush. Not a little bit. Exactly. Then I ran the dehydrator for a little bit, checked on it and it had almost all "melted". After cooling, the liquid that I had been trying to evaporate with the dehydrator was in a little pussle all by itself, and the mystery substance had re-formed crystals, only now it looked more like ice. Much bigger crystals that were longer and big (2 inches square), flat sheets. Very hard.

The stuff that dried while stuck to the side of my jar looks like big salt crystals. So clear and sparkly. They really are nice, just wish I knew what the hell they were....


Pokey the Inept Chemist

 

[amor_fati]

All SWIM can offer is that when reacted vinegar with an excess of sodium carbonate and added IPA, much of the sodium carbonate did seem to precipitate out as well. When he put the mixture in the freezer, it formed a sort of slush in the bottom (sodium acetate may cause this). It's possible that the lye and IPA in the mixture may have cause salts to precipitate out (if lye and IPA are much more soluble). If SWIY thinks there's product in there, just wash with warm heptane.

 

[Pokey]

Thanks amor_fati!

I don't think there's anything good in there, just want to figure out what it is and how I made it happen. Curiousity and the cat you know!

Pokey

 

[shoe]

Your topic makes me think of this:

which was DMT fumarate which swim re-melted. It formed a really dense, flexible goo which smelled lightly of limonene and kinda floral.

 

[bufoman]

I didn't read the other thread but....

Heptane is not a good solvent for extractions of anything. When you put it in the freezer the product is crashing out too fast and forming oil instead of crystals. This happens with heptane and octane. A slow room temp evap may or may not do this depending on what alkaloids are present. The oil will prob eventually form a semi solid as you said but won't be as clean as properly prepared crystals. Try a more polarized organic solvent for extractions as your yield will go up and you will need less. Then use hexane not heptane for crystallization.

 

[Jorkest]

ive used heptane to freeze precip...and got beautiful snow globes every time!

 

[Phlux-]

myself - heptane slow evap gives beautifull xtals - bufo can u explain a bit better why hexane is better for re-x ?