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A/B crystallization woes... Options
 
Global_Roaming
#1 Posted : 9/3/2013 12:25:55 AM
Hi everyone - first up, I want to thank every contributor to this site - its a fantastic resource!

Lately I've tried my hand at an A/B extraction using Q21Q21's vinegar/lime/naphtha tek on MHRB, which has gone well up to a point, where I'm now stumped. I've been researching ad nauseum, but I still can't work out what I'm doing wrong.

When I do my freeze precipitations all goes well - end up with a bunch of white crystals in my mason jar. I lean the jar on its side in the freezer, then after crystallisation I spin the (sealed) jar around and let the naphtha drain to the other side of the jar for several hours in the freezer before pouring off, and repeat this a couple of times to drain as much solvent as I can. At this point, the crystals still look saturated with solvent or condensed water inside the jar. When I remove from the freezer and dry in the open air the crystals melt leaving a white/clear goo of unknown purity. Things I've tried:
- slowly bringing the jar to room temp before opening to reduce condensation
- using a flat pyrex dish in lieu of a mason jar
- air/fan drying (tried both)
- pouring through a coffee filter and then air/fan drying (tried both)
- re-dissolving the goo in warm acetone then slow evaporating overnight

All lead to the same result: a white/clear goo that will not evaporate any further. In my amateur opinion, I suspect that fats/oils are not completing separating during the freeze precipitation process; and/or the high ambient temp (always over 80ºF) melts the crystals; and/or the high RH (always about 85%) saturates the crystals with H2O. I realise that I can still use the goo to make enhanced leaf, but seeing as this is my first attempt I'd really like to ensure max purity and be able to accurately measure doses.

Should I try repeated freeze precipitations with fresh naphtha?
Should I try to defat the the goo with a weak vinegar/water solution then decant with naphtha?
In future extractions should I de-fat the MHRB/vinegar/water solution with naphtha before basifiying?
Do I have absolutely no idea what I'm doing?

Also, I have very limited access to materials/chemicals - the only solvents I have are pure naphtha and water miscible acetone (incidentally, I still can't work out if this means anhydrous acetone). It is very problematic for me to access other common chemicals (eg. fumaric acid, sodium carbonate etc) that are usually available in most places. Any/all help would be most appreciated! Thanks for reading and sorry for the long post.
/peace out brothers and sisters
 
endlessness
#2 Posted : 9/3/2013 1:41:20 AM
Does your naphtha evap clean?

Also, did you try passing a knife or similar around the goo, doing several 'scratching' motions, and letting it stand for a while? It usually starts solidifying. Easier to do this when you have it in a glass pyrex wide dish, and then once it solidifies use a wide razorblade to scrape it up. Sometimes it may stay more waxy instead of dry crystals but it should solidify.
 
Global_Roaming
#3 Posted : 9/3/2013 1:46:59 AM
endlessness wrote:
Does your naphtha evap clean?

Also, did you try passing a knife or similar around the goo, doing several 'scratching' motions, and letting it stand for a while? It usually starts solidifying. Easier to do this when you have it in a glass pyrex wide dish, and then once it solidifies use a wide razorblade to scrape it up. Sometimes it may stay more waxy instead of dry crystals but it should solidify.


Thanks Endlessness, yes the naphtha evaporates very cleanly on testing - no residue, no smell, no trace. I'll give the scratching technique a go. Cheers.
/peace out brothers and sisters
 
wearepeople
Senior Member
#4 Posted : 9/3/2013 2:19:36 AM
What's the humidity percentage where you are?

I've had similar problems when the humidity peaks. And when it does, the scratching method endlessness described has always worked out for me.
+ ---- + ---- + ---- + ---- + ---- + ---- + ---- + ---- DMT Nexus Research ---- + ---- + ---- + ---- + ---- + ---- + ---- + ---- +
 
Global_Roaming
#5 Posted : 9/3/2013 6:46:52 AM
wearepeople wrote:
What's the humidity percentage where you are?

I've had similar problems when the humidity peaks. And when it does, the scratching method endlessness described has always worked out for me.


Relative humidity is usually around 85% - I live in the tropics.

I had some drained, freeze precipitated crystals from last night and tried the scratching method an hour ago - no luck, it seems the more I touch the crystals, the faster they melt (which takes about a minute). I might try an acid wash and then revert back to the flat pyrex baking dish to see if it makes any difference. If all else fails, then its changa all the way Smile
/peace out brothers and sisters
 
endlessness
#6 Posted : 9/3/2013 11:32:23 AM
but do you already have it in the wide glass dish when you do the scratching? If not, maybe use a little warm naphtha to dissolve your stuff and evap it onto the dish

Repeat the scratching thing a few times, maybe have a fan turned towards it.. You should notice the whole thing getting more opaque and hardening up.


As for the humidity thing, I've heard this speculation before but I can't seem to find truth to it, because if you think about it, DMT freebase is insoluble in water. So even if there was condensation or whatever, it shouldn't dissolve DMT. I think more likely its traces of naphtha around that didnt evaporate and keep your DMT dissolved.

But yeah try it out and otherwise re-a/b or changa.

Be well
 
Global_Roaming
#7 Posted : 9/6/2013 7:01:19 AM
HAPPY UPDATE:

I finally managed to dry my crystals! After defatting a new batch of MHRB (yes, I know the consensus is that this is unnecessary for MHRB but I was desperate), then freeze precipitating, draining, upside-downing, draining again and finally putting the pyrex tray into an air-conditioned room under a fan (which brought the RH down from 84% to 52%, and the temp from 29ºC to 24ºC) my crystals are happy drying away. Now all I have to do is explain to Mrs. Roaming why the bedroom smells a little funky...

Thanks for all your help, nexians Thumbs up
/peace out brothers and sisters
 
 
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