G'day fellow travlers
Got Q for you.
Skip too the the sodium carbonate step if you're not up for a long-winded blob of info.

Doing a 400g acacia a/b hybrid (loosely following BLAB tek) and have been trying different techniques out. Before anyone asks, the reason for the large-ish quantity of bark being used is that it was not properly dried when acquiered and had developed a mildew or mold situation. A very fine white powder was appearing on some of the bark (not much though). So i decided to do it all at once before it got any worse.
And i know, mold toxins and all that. It will not be consumed until what is in it is known. Might have a chance to run it through a Mass spectrometer soon, so thats good.
All solvents used are being considered as contaminated as well (even after distillation) just to be safe.
Now thats out of the way, what was done:

-400g of 1.5%ish yielding (tested) finely shredded acacia root bark in a 4L reagent bottle (regular glass) (teflon lid) split roughly 1/3 off and put it in a similar 2L bottle as it was to cramped in the 4L bottle. For the sake of not writing and reading two separate lists i will only talk about to 4L bottle from hear on
-Freeze thawed once
Let sit in 2L of distilled water and 4% vinegar 1:1 ratio, sat at room temperature for an hour or 2
-250g of sodium hydroxide in 500ml of distilled water and was slowly added to the bottle
-swirled occasionally and let sit for 2-3 hours
-1.7L of distilled water was added
250ml of room temperature heptane was added to room temperature base mix
(i usually use 1-2L borosilicate bottles and am not used to such a large bottle so room temp seemed a sensible move)
-Turned the mix end over end for 2 minutes and let separate 8 times
-pulled of 200ml of heptane, filtered and put in -25C freezer for 12 hours
-two pulls like this and a re-x produced 1.090g of beautiful glass shards (never seen it this clean before!) the re-x leftovers was 1.45g of yellowish crumbly wax (yummy)
-At this rate it was going to take a lot of pulls to get everything out of the base mix so i switched to 200ml of d-limonene
-Mixed at room temperature the same as the heptane
Salted out with vinegar and water
-Boiled down vinegar to a small amount
-Added excess sodium carbonate (wet oatmeal consistency), mixed thoroughly and let it sit for an hour.

Now here is where the problem is, at this point i would usually fully dry out the sodium carbonate mush to get rid of water and any traces of d-limonene and pull the alkaloids with 99% IPA, this would produce a red goo (roughly 1/4 the potency of crystals and naphtha extracted goo) that i make into changa that i call Red Limbo
But i thought, 'why not do some heptane pulls first!?'
-So without drying it i put the sodium carbonate mush in a 250ml teflon sealed bottle
-Added a little more water to make it more slushy and added 105ml of heptane
-Heated mix to 50C and swirled for 10-15 minutes, letting separate a few times
-While still at 50C pulled off 100ml of heptane (it instantly turned to milk on contact with cold pipette)
-Put in -25C freezer for 12 hours
- Poured of heptane and dried the crystalline goo (mostly goo)
Now finely, the crux of this post.
Once dry something weird was noticed, the extract smelled strongly of the sodium carbonate/alkaloid mud pie!
A small heptane re-x was performed, leaving behind a lot of goo. After evaporating the heptane roughly 450mg of very gooey crystals were left.
(this is from one 100ml heptane pull from sodium carbonate mud pie)
After this re-x the sodium carbonate smell was pretty much gone,very faint.

I had a search and couldn't find anything on sodium carbonate mud pie smelling contamination

Three theories i have are:
1- Some of the sodium carbonate mud pie was simply suspended in the heptane and precipitated out in the freezer.

2-Possibly impurities in the sodium carbonate that are solubule in the heptane. Never noticed this with the IPA extracted Red Limbo goo, though it has a very strong smell of its own.

3-Whenever i salt limonene with vinegar and separate it multiple time in a separatory funnel until no limonene layer is present, the vinegar smells strongly of citrus.
After boiling down the vinegar the smell is more subtle.
If limonene is slightly soluble in vinegar then it would be in the sodium carbonate mud pie if the mud pie isnt fully dried. That limonene would then transfer to the heptane bringing the vinegar along with it with some sodium carbonate in it. Or would the freebasing negate this from happening since it isn't acetic acid anymore? Sodium acetate perhaps?

I thought of theory #3 after remembering a post by downwardsfromzero.
"I've found this too, limonene - or something similar such as citral - is somewhat soluble in vinegar. It could be that DMT acetate acts like a cationic surfactant, just looking at the molecule.

This also applies to citrates, so it could be that limonene (or citral) is attracted by the indolethylammonium cations."
https://www.dmt-nexus.me...aspx?g=posts&t=68650

Occam's razor would suggest that i am over thinking it and theory 1 is what is at play here. Though when I re-x the weird smells goo I was very careful, minimal heptane at 50C with minimal agitation..
But my knowledge of chemistry is very limited so i can't really say..

What do you reckon?
Thanks for taking the time

Light your path with love
Peace

Ok, so i've done 3 heptane pulls on the sodium carbonate slushy yielding around 2.5g of very gooey crystals. The smell that was thought to be mostly gone after a re-x turns out to still be quite strong but not as strong as before the re-x. The smell of the extract was overpowering the sodium carbonate mud pie smell but after sitting in open air for a while the extracts smell was not as strong.
I am currently fully drying out the sodium carbonate mud pie and am going do my usual IPA pulls on it. Doing the same with the extract already pulled from the mud pie.
Once fully dry im going to take some of it, rehydrate it with water and do a heptane pull to see if the smell still comes over.

Could someone clarify what IPA is for me? Cause I'm thinking India Pale Ale.

Isopropyl alcohol.

Edit: I'm not sure how tasteful jokes about pederasty are. I know it's Big Lebowski quote, but still...

Update:

Ok, so this whole extraction has been quite irritating, a testimony to the 'when scaling up, scale it down. Should have just done acid boils and reduced it in the first place.
I was worried the mold might have developed further if I didn't get it in a highly basic solution asap.
Oh well live and learn.

Anyways, the sodium carbonate mud pies were re-done and this time were fully dried in a food dehydrator and air dried for days until powderizable.
The mix was pulled with ipa, the ipa was distilled off and the extract fully dried.
The resulting goo (3.5g) was washed with 100ml of heptane at 60C on a hotplate stirrer for 1 hour.
Some sodium carbonate settled out, left it in a hot water bath for 30 minutes to allow any small particles to settle to the bottom.
While still hot the heptane was carfully decanted from the sodium carbonate, the heptane instantly turned to milk in the pipette. Did a few more small heptane pulls to get whatever was left.
Put them in the freezer (-25C) for 12 hours.
Poured off the heptane and dried the crystaly goo. (There still seems to be a bunch stuff in the poured off heptane, will distill off the heptane and dry whatever's left.)
Result of the freeze precipitation was 3.2g of goo and crystals.
Now, I think I made a miscalculation of weight in my previous post when i said the contaminated goo weighed 2.5g. I either weighed it wrong or their is now 1g of something else in there...
Next the 3.5g was fully dissolved in a minimal amount of heptane, dried and then fully dissolved in a minimal amount of ipa so if there was 1g of unknown impurities it would have shown itself to some degree so I think I just miscalculated the weight.
That aside the sodium carbonate mud pies smell is gone. Not fully drying the sodium carbonate mud pie in the first place was what caused the problem.
My "3rd theory" seems to be what was at play in some way.
D-limonene and vinegar seem to be soluble to some degree, enough to cause an issue like I've had.

I would love some expert input on this to give a chemical explanation even though it would baffle a muggle like me

I hope this post can help anyone who runs into this issue or prevent it from happening.

Peace oott