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A/B using lye and naphtha. Filtering is easy! Options
 
Homo Trypens
#1 Posted : 10/31/2020 11:59:07 PM

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When i first started extracting, i did an STB and two A/Bs. Since then, i explored the world of lime/d-limonene teks and never performed another A/B, so i decided to revisit it. Because the first result looks really awesome quality-wise, i start this thread with a description of what i did.

Ingredients used:
- 255g of powdered MHRB
- 6L of H2O
- ~70g of sodium hydroxide
- naphtha (Wundbenzin from a german store)

Equipment used:
- a large enough pot (mine is 9L, probably 3L would've been enough)
- something to stir
- a coarse strainer
- a fine strainer
- 2 containers 3L each
- a 10ml pipette
- a freezer compatible glass dish
- a magnetic stirrer without heating
- a 1L bottle with wide wouth

1.) The Tea:
I boiled 255g of MHRB powder in 2.5L of water for 30min. It was a full but not a violent boil. I recommend stirring regularly to avoid bark getting burnt in the bottm of the pot.
I then poured the liquid into one of the containers, through the coarse strainer. when the strainer filled with bark, i put that back into the pot, then continued pouring. It was about 1.5L of tea. I added 2L of fresh water to the pot and put it back on the stove.
After another 30min, i poured the liquid from the first container through the fine strainer into the second container and put the solids back into the boiling pot. I filtered the tea from the pot into the first container through the coarse strainer. I added 1.5L of fresh water to the pot and put it back on the stove.
After 30min more, i strained the tea from the second boil through the fine strainer into that of the first boil. i washed the now empty container and filtered the combined tea through the fine strainer into it. I filtered the 3rd boil through the coarse strainer.
I let everything sit over night now. That allowed more finer particles to swell to a filterable size, and for a tannin sludge to precipitate at the bottom.
I washed the pot and filtered all the teas through the fine strainer into it. I put it on low heat to start reducing. I recommend low heat, can even be below boiling, because that allows a tannin skin to form on top, which can be removed from time to time. In a hard boil, this skin gets ripped into pieces constantly and might make trouble later on.
I reduced the roughly 3L of combined teas to 0.7L and filtered that through the fine strainer into my 1L bottle.

2.) The Soup:
After a little bit of cooling, i added lye to it. I added in increments of 1 spoon or around 10g. After every spoon, i waited for a few minutes before adding another one. I was so cautios because the tea was still quite hot by itself.
I had measured 200g of lye, but when the familiar white/milkyness and consecutive blackening in the soup occurred after just 2 spoons, i stopped after adding around 70g.

3.) The Pulls:
I added ~100ml of naphtha to the bottle, inserted a stir bar and placed it on my magnetic stirrer. It was still very warm. I let it stir for 1h, then i pipetted off the naphtha into the dish (via another glass container, to ensure no lye soup droplets make it). I wrapped the dish with 2 layers of cling wrap.
I added fresh naphtha to the bottle and continued stirring. The tea was now at room temperature.
I placed the dish into the fridge for 2h, then moved it to the freezer.
8h later, I took the dish out, and there was a lot of crystals. I removed the wrap and poured off the naphtha into some glass container, slowly, so all the crystals stayed sticking to either the glass or other crystals. I placed the dish back in the freezer, upside down, with the wrap back on, for an hour. Then i took it out, let it warm (still upside down) to room temp before removing the wrap. I then placed it in the open standing on its side, so vapors can leave but dust can't get in.
A few hours later, i scraped off most of the crystals. I used something soft, which didn't get everything off.
What came off looks super pure, but it is only around 100mg (if my scale can be trusted - not sure atm). My assumption is that i didn't leave it in the freezer long enough, and that i should have used a rigid tool for scraping. I couldn't find one at the moment. I ended up redissolving the rest in the naphtha from the first pull.
I pipetted the second pull into the dish at this point (yes, after many hours of stirring), and put it into the fridge, tilted so that half remained dry. I added the naphtha from first pull back into the soup bottle for a third pull.
After about 8h, some pretty large crystals had begun forming, the dish was still in the fridge. I decided to get the third pull and add it in there. I very carefully tilted the dish to the other side, so the crystals were out of the naphtha, added the naphtha from third pull, and tilted the dish back so the crystals were submerged again. I placed it back in the fridge for a few hours, then moved it to the freezer. I will leave it there for at least 24h this time.
I added fresh naphtha to the bottle, going for a fourth pull. This time, i used a long stick to manually disturb the soup/naphtha sporadically, in addition to the permanent magnetic stirring. I will keep up this regimen until the dish is availbale again.


I will update with pics and weights once they come in Smile
Homo Trypens attached the following image(s):
tea.jpg (14,891kb) downloaded 174 time(s).
soup.jpg (3,269kb) downloaded 171 time(s).
flakes.jpg (115kb) downloaded 170 time(s).
 

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tripwire
#2 Posted : 11/1/2020 7:35:51 AM
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Lovely work HT.

I would like to emphasize that the ratios of bark to water used here must represent the absolute minimum amount of water needed to not cause losses in dropped tannins.

I think HT confirmed that the final 0.7L was not allowed to cool fully before basing, as cooling (for decanting from sediment) may have pushed things over the edge precipitating tannins that tangle up actives (even if solution were acidic!). For the inexperienced extractor I would recommend reducing to 0.95L to leave 50ml for solvent which is more than enough for an extraction this size.

I have played around with acid boils and washes and never been able to successfully reduce to a manageable volume without precipitating out tannins and taking losses. The reddish sludge that precipitates first is probably clear of actives, the blackish tars which come after further reducing almost certainly contain actives.

Great job HT in making the acid/base approach work. To the reader of this tek, follow instructions exactly or reduce less aggressively, do not undercut HT's numbers/limits, this is as good as can be done with mhrb and its terrible and sticky tannin content.
 
Homo Trypens
#3 Posted : 11/1/2020 3:15:44 PM

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The combined pulls 2 and 3 are now back out of the freezer. It was a better amount this time, 600mg of beauty. Still pretty low for 255g bark. I'll keep pulling until nothing precipitates anymore, then pull once more with d-limonene. In case total yield ends up being too low (<1%), i didn't throw away anything. We'll see where the DMT is trying to hide Smile

In my mind, possible explanations for my low per-pull yields are:
- boiling without any acid didn't get all the actives out of the bark
- my magnetic stirrer doesn't create enough contact for efficient pulls
- because i didn't evap any naphtha before cooling/freezing it, it won't release all of the dissolved goods

I am prepared to test and remedy all of these hypotheses. If necessary, my planned steps are (in this order):
- In any further pulls, apply some manual agitation in addition to the mag stirring
- distill off 90% of the naphtha, do freeze precipitation with the remaining 10%. Then evap that, too.
- do an STB on the 'spent' bark and sludges.

I have pipetted off the 4th pull, after adding all the used naphtha from the freeze precipitaion and stirring about 2h more. It sits in the fridge now, will move to the freezer tomorrow.
Homo Trypens attached the following image(s):
crystals_collage.jpg (1,311kb) downloaded 154 time(s).
 
downwardsfromzero
#4 Posted : 11/1/2020 10:59:49 PM

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Lovely crystals! Drool

Quote:
distill off 90% of the naphtha

If you end up doing this it would be interesting to see if any DMT co-distills with the naphtha.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
 
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