Hello all,

I recently tried to perform an A/B extraction on 250g of ACRB.
Reagents used:
-250g powdered acrb
-lab grade sulfuric acid
-food grade sodium hydroxide
-lab grade hexane
-both distilled and filtered H2O was used interchangebly
-sodium sulfate anhydrous (used for drying warm solvent pulls)

I believe that is all the important stuff listed.

To prep:
-Initially lysed the acrb with freeze/thaw method (1 time)
-3x Acid boils with sulfuric acid (pH aprox. 1-2)
-Reduced
-basified with sodium hydroxide (pH 13-14)
*I usually try to reach a pH of 'nearly' 1 or 14
-2 pulls with aprox. 200 mL of HOT hexane
** Instinct tells me the excessive heating of hexane is the cause of the red precipitant

So prior to adding the first 200 mL of hexane to the basic aq. solution, the hexane was nearly boiling, and the aq. sol. was very warm as well.
After adding the solvent and mixing, the combined heat caused the hexane to boil inside the flask. Obviously, it was allowed to seperate, albeit not long enough, and mixed a few more times.

When I decanted the original hexane pull it was a dark amber/yellow color.
A second pull was done - similar results.

So I figured I dissolved a lot of fats with the boiling hexane, and decided to dry the combined first and second pull with sodium sulfate anhydrous to try to catch any of the tiny particles of aq. sol. in my NPS.

This was done with relatively good results clearing up the hexane to a more seemingly 'normal' light yellow color.

I then poured the *warm* hexane through a coffee filter and into a glass dish.

now keep in mind at this point my NPS was no longer showing signs of the amber/red color.
After covering and allowwing to cool to room temperature for several hours, i returned to find strange double helix shaped red slime gathering on the bottom of the dish.

it continued to cool and freeze/precipiate for approx. 12 hours

here are the results..

1st and 2nd pic are original freeze/precip.

3rd is a re-x with heptane.

My question is, I have been reading mixed things on red precipitants, and I realize it is some sort of contaminant, but I find it strange that it seemed to precipitate out of nowhere, especially with the extra step of drying the first pulls, which is something I usually save for re-x's.

any input would be great on what you all think caused this to happen..

Interesting tek and interesting result. Betacarbolines maybe?
Looks very much like jimjam that gets pulled from mhrb..

Do you have access to reagents? A couple of the extracts in the acacia analysis thread came out red..

Interesting, this is the first time I have heard of jimjam, and I couldn't agree more, the scrapings came out very very dark (like the jimjam) compared to other honey-like 'goos' this plant has given me.
and unfortunately, I do not have free access to analytical reagents/equipment at the moment.

I saved a small amount of the original scraping, and plan to report the effects after testing it out.

Its amazing how many different variables play into the outcome of the extract.

Regarding the lab I used - I pretty much just used a mash up of everything I have done in my org. chem. lab, and the guidelines layed out in joshisom's, and cyb's add salt, which were incredibly helpful in early research of this process.

I had the same in my first mhrb extraction. First i thought i contaminated my naphtha with basic soup but after cleaning the spice same amount of it was still present in final yield.
Jimjam you say a?

Another thing you could try is dissolving in alcohol and seeing if everything is soluble, if there is any remaining particulate that won't dissolve in the alcohol filter it out.

When doing the acid cook, I think pH 1 shouldn't be needed, pH 4 is good enough.

Before drying the nonpolar, it may be useful to leave the nonpolar in a warm water bath (keeping the nonpolar at the same or higher temperature as the extraction was done at) for a while to let tiny water droplets and particulate plant matter precipitate, then decant (optionally dry and decant,) and finally cool and freeze. Simple precipitation in the still warm solvent can be a very effective and efficient means of cleanup.

When the crystallized product has been properly dried, you shouldn't need to again dry it after redissolving for a recrystallization, provided that the solvent is dry enough.

Using hexane for the initial extraction can be bothersome due to its low-boiling nature. I use naphta that boils from 90 to 130 degrees Celcius, it's also far cheaper than lab grade hexane. The hexane is nice for recrystallizations though, as I find it to be more selective as a solvent. It seems that longer chain alkanes are better solvents for fats and waxes.

- Yes! I have found this to work wonders, also, even just letting the warm solvent sit out at room temp for about a half hour after the pull seems to allow for some of that excess fat to fall out.



- thanks for pointing that out, I would typically save the sodium sulfate for when i use vm&p naphtha as my NPS, and not waste it on the hexane, but when i saw how dark the pull came out to be, I was caught off gaurd and immediately went into purifying mode, lol.

And I assume that store bought naphtha doesn't really require drying everytime, but then again, it shouldn't hurt anything either



- I haven't read very much into this process, but it definitely sounds like it would be worth looking into for future extractions.




Thanks for all the input!

If you have the proper lab equipment, do distill any store bought solvent if you can. Some OTC chemicals are really nice and clean, some are really loaded with crap.