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Alks or by products?

Yuxibu

Established member
So I won't be stating numbers for obvious reasons but let's say due to logistical reasons this time I decided to extract double the amount I usually extract from. but since I only had a small mason jar I ended up concentrating the aqueous solution quite a bit. (Same volume I normally use for half of the bark.)

Proceeded as following
4x 1h30 boils with citric acid
Reduced combined boils to 450ml
Added 30g of salt
Added 90g of naoh
Pulled 4x with 100 ml heptane

While pulling I was putting most of the content in a main jar, and the few bits that came with some basic soup in a narrow mouthed spice jar that had a some water with a pinch of sodium carbonate.
With that I managed to easily grab those last bits of heptane and passed it to the main jar, but during that process noted there was a big clump in the spice pot so I retrived it with a small spoon, washed it with water + sodium carbonate and the result is what is presented in the attached picture.

So to recap that spice jar had:
Water + sodium carbonate, and some small amounts of bark soup with sodium citrate, salt and probably some unreacted naoh, since I used a generous amount.

So at first glance, looking at the picture does it look like some alkaloids precipitated due high concentration of the soup, or is it just a blob of byproducts that clumped together?

How would you proceed to further test and eventually clean this clump while avoiding alkaloid loss?
 

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I'm no expert, but mini A/B sounds like the route to go here ... dissolve in vinegar (might take a while and need some breaking up and stirring well), filter off anything insoluble, basify and pull.
 
All my nps is in the freezer atm, I'll need to wait a couple of days to do that.
I broke it into smaller chunks and patted it dry, it smells mostly like lye but there's some faint indole scent.. might be solvent leftovers though.
 
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