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Failing A/B - Need a Little Help Please

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Bill Cipher

Bill Cipher

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SWIM has performed a couple of A/B's in the past with very healthy results (both in terms of purity and yield), so he's utterly perplexed as to why his current kitchen project isn't behaving as it should. Any advice he can get to help save his troubled extraction will be appreciated.

Anyways...

Started with 1kg Celestial Source pre-ground. It's the brand new stuff (touted to deliver between 1.2 and 1.4%), so he can't imagine his source material being the issue. Performed his normal Marsofold tek with a couple of extra steps. Did 3 separate boils with 3 parts distilled water to 1 part white vinegar (ph between 3.5 and 3.9 throughout), then froze the wrung out powder rock hard over night and did one final boil the next day just for good measure. Decanted and reduced (over a very low flame) down to about 3 litres, then defatted with 3 200ml limonene pulls while still in the acidic phase.

Based up the soup to ph 14, did 10 hot 200ml naptha pulls (but did not heat the jug at any point). Rolled/swirled/turned end over end for maybe 5-10 minutes each time (with a clean break on every one and little to no emulsions) and ended up with a big-assed jar of pale yellow naptha. Did 2 50ml carbon washes with ph 10 sodium carbonate water (drained within probably 30 seconds), one more 50ml distilled water wash (also drained very quickly) then dried with a good sized pinch of microwaved epsom salt (filtered very quickly).

Put the entire 2 litres of now 100% clear naptha in the freezer and got bupkis (or practically bupkis anyway - a very small amount of crystals clinging to the bottom of the bowl), so he evaporated roughly 70% with a fan blowing over the top, expecting to see snowflakes floating throughout, but all this seemed to do was bring the yellow tint back. There are dried crystals encrusted around the bowl where the solvent has evaporated and a very few slightly dirty looking floaters, but this is about it. The remaining 30% is now back in the freezer for about the past 4 hours and there is very little to show for it.

So what gives, extraction professionals? How does my octopus friend salvage his project? Is it possible that carbon washes or a tiny amount of epsom salt could have eaten up his spice? Could the solvent still not be saturated enough? Is the fact that it yellowed up as it evaporated an indication that the goods are actually in there?
 
SWIM thinks that the carbonate stole your DMT maybe. PH 10 far above the PKA of 8.5 or something. Hope you didn't throw it out.

SWIM thinks that your naptha is plenty concentrate for precipitation.

Good luck.
 
There is a rumor floating around that CS has had some garbage bark recently. I have no firsthand knowledge of the validity of this information, I only know that when I posted some problems that my octopus friend was having with an extraction, the first question from another helpful nexus member was "Did you get some of that shitbark from CS?".

I hope this isn't the source of your troubles. Everything in your post seems perfect to me and your octopus friend should be swimming in spice so to speak:wink:

Pokey the Empathic:cry:
 
No, this is from their latest shipment. Supposedly, whatever issue they briefly had had been remedied by the time of SWIM's purchase.
 
I have never followed that exact procedure so not sure exactly what happened. I would reduce the solvent voloume at least 50percent or until cloudy and try freeze percipt again.

I almost hate to speculate do you still have the carbon wash? That is a lot of bark you should be seeing something even if it is weak.

(1) Hopefully reducing the solvent and try freeze percept will tell the tale. If you are super curious you could evap some of the solvent real fast with a fan and see what remains, that may allow you to breath a sigh of relief and wipe your brow.

(2) Bark could be weak or BUNK.

(3) carbon wash removed spice

Those would be my top three, the other things you describe should not have caused any issues that I can identify.

Good luck man I hope its #1 let us know.

I currently have the opinion that all the tricks that help clean up a A/B do help but may be time consuming to the point of being compulsive. (I BEEN THERE Done That)

A good defat in the beginning combined with a definite plan to recrystallize to transparency in the end, to me seem much faster and the result is in no way inferior to "Every trick under the SUN a/b method". I have spent half my life filtering MHRB solutions to resemble red wine or dark tea my recent experiments seem to point to overkill.

I have done a few single pot A/Bs lately with just a defat in the beginning and the final solvent pulls in the end being the only fluid transfers in the ENTIRE A/B process, thats right no filtering of plant solution.:shock: I just do a decant at room temp and allow solution to settle between pulls.

Of course recrystal of final spice requires normal filtration and seperation/removal of CRAP at the bottom of warm solvent before dmt percipates the standard re X procedure.

All may feel free to try the Lazy A/B themselves I would be curious to hear others outcomes and thoughts on this. Type up a tek if you wish.

I can hear the Ant man chuckling in Hyperspace now:lol: The race is on and it looks like its the Classic Turtle and the Hare battle.
Pretty exiting if you ask me:lol:

see you there
Peace
MV
 
Yeah, that's the deepest cut for sure - being outsmarted by Captain Gratitude. He did take pity on me today, however, and benvolently laid a few measley crumbs of his handywork upon me. So all I can say is "Love and Gratitude". Or "Hugs, Peace and Chicken Grease". Or "Kittens and Moonbeams". Or something. I'm not sure. But I'm open to catch phrase suggestions.

Unfortunately, I didn't keep the carbon water. It just didn't occur to me - went straight into the sink. The consensus opinion around here seemed to me that too high a ph wouldn't present an issue. I wasn't really aiming high - a little just goes a long way.

I'm wondering if it could be the epsom salt. I strained it through a coffee filter, but not all of it came out solid. How a little bit of residual epsom salt could eat up 12-14 grams of spice is a mystery to me, but I'm no chemist.

I knew the whole tek was overkill, honestly - I was planning on multiple re-crystallizations as well. I figured I'd live with a loss of yield and shoot for glassy perfection. It never even occurred to me I could somehow end up with nothing.

What a drag.
 
sodium carbonate would NOT eat your spice, but the last pure water wash would possibly! I would avoid doing this last non carbonate wash

Another issue is indeed the excess solvent.. I would wait overnight to see if anything comes up from what you have so far, otherwise I would evap it till its VERY little, like 100ml total or smt (ah what a waste of naphtha.. go limo! :p ), and stick in the freezer again.. At this point I guess thats all you could do...

Next time I would say do only one sodium carbonate wash (with pH around 10 I would say), not necessary for more, specially not the pure water wash....

Also one important thing I think could have been part of the problem, Ive noticed 3 boils are usually not enough.. I recommend doing like 5x mimosa boils.. Maybe you didnt catch all the stuff there.

but lets hope something does come out when you have like 100ml left in the freezer... good luck
 
Since your total wash was three 50ml=150ml to that huge amount of solvent and you do see a small amount falling out I bet there are multiple grams of magic in there. Things may be no were as bad as they seem now.

If it was me I would have the solvent out of the freezer in a pan with dust screen on top(called splatter screen in cooking prevents grease from spattering when frying. cheap at Wallmart) on a heating pad with a fan on it. Till cloudy then back in the freezer stuff will start to drop out in a couple hours max.
 
The first problem I see here is the amount of cleaning steps you did before putting the naphtha in the freezer. You probably lost most of your spice to the "cleaning steps"....

I doubt that it can be recovered. I would not use the limonen stuff for a defat, it seems to be able to suck up damn near everything. I would not do a carbon wash before crystalization...MAYBE as a clean up afterwards, but truly I think it is 100% unnecessary.

I would in fact, take out ALL of those cleaning steps save the defat (but only if you are going after extremely pure spice). I would change out d-limonene for hot naphtha or Toluene/Xylene.

Everything else you did looks pretty sound. The salt did not interfere with your yield. I've poured in A TON of salt (NaCL as well as epsom salt) without loss of yield.

Your bark MAY be bunk, but even with really bad bark you should have gotten better yields than you did.

Clean up, for the most part should be done AFTER you have your xtals. Recrystalization is a very quick and easy way to get very pure spice very quickly. Room temp rextalization is even better.


Yeah, REMOVE all the clean up steps and you will probably have the yields you are looking for. Sorry about this extraction my friend, I think it's a gonner.

Not to be hard on you, but there is a reason that everyone spends time at the end of their extraction cleaing up their spice. A defat is almost overkill, what you did...wow man...just wow. I get the reasoning behind it I think, but in practice it was just too much. Remember each clean up step inevatibly drops your yield a bit.

When experiementing on new methods of xtraction it is always advisable to use 1/4 or less of your total mimosa.
 
This is a pretty good representation of my overall personality, actually, and a definite illustration of my neuroses in action. I've always subscribed to the global theory that if one = good, then four = better. My reach generally exceeds my grasp, and while this has lead to me getting my ass handed to me on any number of occasions (both literally and figuratively), it's also allowed me to achieve a couple of cool things in between.

Every step in the process seemed pretty sound, in and of itself - I guess I just strung a few too many together. I was shooting for a shoot-worthy end product, in case Ant and I got to feelin' saucy. Like I said, it really didn't occur to me that it could all just up and disappear.

Still, things are not quite as bleak as they appeared to be yesterday. After the initial evap, my precip did yield something, and I believe there is more spicy goodness slumbering away in the solvent at present. I'm evapping again, probably down to 100mls or so (per Endlessness' suggestion), then I'll freeze precip one last time, and maybe try a couple more pulls. The yield will be piss poor for sure, but I think I'll salvage a few measley G's. The loss of 80 bucks won't kill me, and I learned a valuable lesson. The week spent in the kitchen stings a bit more, but next time I'll knock the fucker out of the park.

Live and learn, my spicy friends. It's the journey, not the destination.
 
Uncle Knucles said:
Decanted and reduced (over a very low flame) down to about 3 litres, then defatted with 3 200ml limonene pulls while still in the acidic phase.
Click to expand...

Hmmm, after all that reduction, I'll bet that the vinegar boiled off to a large extent leaving a much less acidic solution. That would mean that the limonene pulls would grab a whole lotta spice.:shock:

I'll also bet that you still have that limonene containing spice.8)

Try an acid wash of the limonene to recover the goodies.:)

Hope I'm right:wink:

OF
 
That actually sounds like a feasible explanation. Chemistry types - would DMT be soluble in limonene at a ph somewhere between 4 and 7? And I was under the impression that vinegar (mostly) remains, while it's the water that boils away more quickly during reduction. Am I wrong? And if this is the case, wouldn't it drive the ph even lower?

Sadly, this is all pretty much academic at this point. The only things I didn't save were the limonene and carbon water. Go figure.
 
I second what acolon says, your going overboard with to many steps to reach the final phase of having the extracted goods. Don't go over and over your solutions with so many washes and things, keep it simple. If your obsessed with getting a final purity do it with a re-crstalization method, or redisolve your goods in a solvent and then wash it as a concentrate, and save every thing, each step, until your sure what's what. In other words complete the basic extraction first, then move on to fine tooth comb purification as a secondary process.
 
Uncle Knucles said:
That actually sounds like a feasible explanation. Chemistry types - would DMT be soluble in limonene at a ph somewhere between 4 and 7? And I was under the impression that vinegar (mostly) remains, while it's the water that boils away more quickly during reduction. Am I wrong? And if this is the case, wouldn't it drive the ph even lower?

Sadly, this is all pretty much academic at this point. The only things I didn't save were the limonene and carbon water. Go figure.
Click to expand...

I have yet to jump into the limonene revolution so I am somewhat speculating in this.

But "somewhere between 4 and 7?" between 4 and 7.2(usually) that is a acidic solution if that amount of solvent will hold over 10grams of spice seems unlikely to me but could be wrong.
Chem guys please fell free to correct me! I am far more interested in facts that can be proven as opposed to preservation of my ego.
I enjoy being wrong because that means I learned something.

I bet a $hyperDollar(have you not heard its the new currency in Hyperspace) that you got a few grams in the solvent. Could be wrong. Let us know


Peace
MV
 
Uncle Knucles said:
Every step in the process seemed pretty sound, in and of itself - I guess I just strung a few too many together. I was shooting for a shoot-worthy end product,[
Click to expand...

I had a funny feeling that's what all the purification steps were for.

Aboslutly do an A/B on the mimosa. I wouldnt put anything from an STB anywheres near a vein...ever...ever....ever. A defat or two in the acidic stage and at LEAST two freeze precipitations AND a room temperature recrystalization with heptane, and a long dry time is probably as close as you are going to get to 99.9% pure DMT.

Activated Charcoal will pull out any off colors, but if you do the extraction and purification as stated above you will end up with crystal clear spice, not white, not yellow, not red or brown or blue or pink, but CLEAR....If you have clear spice no carbon wash will be required. In fact, no wash at all will be needed if you do 3 crystalizations on it.

PM me if you want me to go over the best ways to recrystalize spice.

Add acid of choice to convert back into a salt, and volia!
 
If you want to learn all about recrystallization and purification of crystals, here is a slightly interested yet very informative video: Rescrystallization. It is the 9th video. This was not found by me, this is posted in another thread by SWIMfriend.

Hope this helps you out. :d
 
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