knowing enough now to ask a few questions

[taz]

hello.
I am beginning to learn the process of an A/B extraction using Acacia.
I've read a lot of forum posts and teks to try and learn the fundamentals -
but I'm still stuck.

while I can sometimes precipate fat crystals at room temperature, I'm unable to keep them.
I have freeze precipated, but am not clear if its needed.
I acid cook, evaporate, basify (watching the brown go to grey then black), and add hot solvent.
repeat. pull the solvent off. set aside and wait. pour off the solvent for later use.
add a small amount of warn solvent, plus some basified H20 to wash any of the polar inpurites.
then .. the crytals dissapear, and DO NOT recrystalize after I seperate the wash/solvent.

I figure that I shouldn't throw anything out - since they didn't just vanish.
I think I understand the relationship between the solvent, heat, ph, h20, etc ... but still fail.

A few questions on what I've seen but not understood:

1. Is the "oily sparkly" stuff floating on top of the basified H20 - the stuff I want?
2. After a solvent/water jar is not seperated - it looks like it floats on top of the polar layer.
Does it degrade anything if left in contact with base?

3. The ratio of water to solvent:
Are there mins/maxs not to exceed or go below?
Can you have TOO much solvent?
Can you wash the base too many times?

4. Heat: How hot can I take it. From what I understand, the boiling point of the product is above 212. Does that mean I can't destroy it in boiling water?
Same for extraction - is there a max temp during solvent pulls?

5. Are the needlelike glassy things that clogged up my seperatory funnel what I'm after?
This sank to the bottom of a big jar I had let sit. I assume its what I'm after.

I have (had) about a half cup of them, and on the last "wash" to try and clean them ... they vanish. My heart sank, and I keep mixing it all back together and trying to coax the creatures.

Any answers or links to forum posts I might have missed, would be greatly appreciated.

 

[3rdI]

after you have pulled the solvent you either need to completely evap it to give crystals, or freeze precip it to give crystals.

which tek are you following?

 

[DreaMTripper]

I think the best way for you to reveal what is there is to do a straight freeze-precipitate without any clean up steps. Yes the oily stuff is most probably alkaloids that are in liquid form. Rather than cleaning them with basic water (NMT in acacia is slightly soluble in basic water so you may lose a significant proportion if the NMT : DMT ratio is weighing more on the NMT side)
There is no need to use high temperatures 40-50 should be more than enough as demonstrated in cybs teks. High temperatures will make NMT more soluble in basic water and can also make gunk migrate to the solvent even if in micro-particles.

 

[taz]

3rdI -

Unfortunately, I'm using a combination of TEKs.
The latest one I'm "following" is Cybs Hybrid ATB tek.
Before starting - I read and compared many TEK's (not all on nexus), to see if there were some underlying fundamentals. Because the temperatures, amounts, procedures were different for each one - it seemed that many of those were just what happened to work for somebody.

There are some parts of the process I'm still unclear on:

**Freeze Precipitation**
Is it required?
crystals formed at room temp over night are more pure than frozen?
freeze precipitation is best accomplished by alternate freeze and warming?

I've gotten large formations after 10 - 12 hours at room temp and then lost it during washing/recrystallization.

** recrystalization /cleaning**
in the past, I poured off the solvent (VMP naptha), collected the flakes - and during the "washing" stage (using basefied H20) -- they vanish.
can you wash after things have crystallized?
can the base water be colder than the solvent, to encourage precipitation?





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[taz]

I think the best way for you to reveal what is there is to do a straight freeze-precipitate without any clean up steps.
* I'll give that a shot.
I'd separate well, freeze for 10-12 hrs, pour off solvent, air dry remains?



Yes the oily stuff is most probably alkaloids that are in liquid form. Rather than cleaning them with basic water (NMT in acacia is slightly soluble in basic water so you may lose a significant proportion if the NMT : DMT ratio is weighing more on the NMT side)

* So don't wash with H20 at all? Perhaps that has been the issue with the "vanishing" crystals.



There is no need to use high temperatures 40-50 should be more than enough as demonstrated in cybs teks. High temperatures will make NMT more soluble in basic water and can also make gunk migrate to the solvent even if in micro-particles.

* what ARE the effects of high temperatures up to 100? (either in the acid cook phase or pull phase)


I'm trying CYBs TEK now .. and have solvent with fat flakes at room temp.

What next?

*** UPDATE ***
I have finally achieved fluffy white goodness!

I used:
Room temperature precipitation
No evaporation
No defat step
Buchner Funnel/Vacuum Flask/No Filter Paper
(vacuum assisted with a shop vac)


Lye and Salt are both water soluable(?) - so as long as I completely separated the liquids, no chance of either of those in the almost cotton/crystalline looking stuff??


Still have many questions about the process:
So far ... the CYB tek flowchart, is the easiest to follow for me.

I'm still winging it with proportions, wait times, etc ... but I think I got the basics down.
Failing so many times initially has given a good idea of what didn't work.
Now ... if I could just remember what that was.

So many ways to look at something, yet its only one thing.

 

[3rdI]

just follow the tek. mixing up teks when you dont know what your doing is why many people fail.

cyb's tek is tried and tested, just do what it says

 

[taz]

I agree completely.
Had I started the process with CYB's tek ... I would have followed it.

I started with one TEK (not from here) ... that dealt with 1kg of ACRB and no defatting.
Needless to say - I wish I had started with a smaller amount.
After I reached out for some help - I got another tek that had defatting with Toulene.
Still no dice ... but at this point I had a LOT of liquid - so I needed to understand the mechanics of it in hopes I could recover from the first two fails. I also realize how nasty Toulene is.

I was only deviating from the TEK's because they were inconsistent and hadn't produced results.
(mind you, I have no idea what the end result looks like - or its effects)

I'll continue with CYB's tek, but would still like to know more about the physics behind it - so I can bend the rules if needed (like rescuing a batch started with another process)

For instance - I did skip a couple steps in the CYB tek - and still pulled fluffy white.
I'm guessing that if it's "fluffy white" at the end, the specific path I chose isn't as important?
(unless I want to replicate it)
****
DISCLAIMER: I am not trying to be a douche by not "just following" a proven TEK. Just trying to better understand each of the steps in the TEK, and what upper and lower limits there are. With so much conflicting information between the various TEKs, it left me a bit confused.

Now I need to learn how to vaporize this stuff and get down to bizness.
I've been waiting on the tarmac for too long, and am ready for take off!