New approach

[GreenDMT]

Hi Nexians
Swim is thinking to do another approach of extraction. He is doing STB soup after pulling with toluene all goods, making reverse A/B with citric acid, and after making base again leave it in base solution to precipitate few days, after spice is making conglomerate. After few days filtering crystals washing with water to remove all base soup and mixing with naphta and washing naphta again with water to remove all polar things. What do you think ?

 

[downwardsfromzero]

What do you think ?

I think you should write out the method more clearly. What exactly is new about your approach?

It doesn't sound too new or ground-breaking so if your methodology is up to scratch there's no reason for it not to work. But make sure you write it out clearly in list form, otherwise it's a bit hard to critique.

Plus, there's no need to SWIM round here.

 

[GreenDMT]

Thank you for pointing me for steps, it's somehow mostly in my brain, but I will try to point it.
step1
100 powdered bark was put in 1/15/1 water/Naoh (I found only concentration of 75/25 of lye and salt)
step2
washed with 60 ml toluene per pull (5x) and all pulls were combined
step3
solvent was mixed with 12% citric acid after this solvent become cloudy (now also it is, but now I figure out maybe is frome water in toluene, it works for the naphta, but the it was very low concentration,until I get somehow toluene)
step4
to the citric solution was aded sodium carbonate solution until cloud appeared, left it seat for 3 days to form some kind of clumps of precipitate which was then filtered and washed twice with water and left it to dry.
step5
dissolving all precipitate( there was split in 2 parts,second was much white than first) with zippo, washed again with water and after put in the refrigerator
now trying to retrieve more from toluene (spice is very soluble in toluene) and I don't know how long it take to transfer in acetic solution). I didn't sow this on forum which are enourmous
Kind regards

 

[Jees]

No 'New approach' , the title is misleading imho, it's a conglomerate of existing steps.
GreenDMT, what do you find yourself 'new' in your menu?

 

[downwardsfromzero]

Welll, GreenDMT, it's good that this hybrid approach seems to work. What were the yields like?

The precipitation of solid freebase from aqueous solution is a less-used method. What inspired you to try this particular variation? Were there any particular tricks to it? Why did you not just pull straight into naphtha from the sodcarb based aqueous phase? Surely if you obtained solid freebase as a precipitate from the aqueous phase it would be usable with a water wash - although I suppose naphtha is quite good for producing decent crystals?

 

[GreenDMT]

The new approach was direct filtering. I was thinking of this mess because I couldn't find decent naphta to extract from base solution, plus if filtrate is dry it is more soluble in naphta without water. All what I have is toluene plus a lighter fluid which I used long time ago but now seams not working, that's why I try to avoid water migration from base soup to naphta, I just filter, wash with a lot of water and then dissolve into naphta. The yield was quite low, 0.7, but I use a source which is not so high.

 

[downwardsfromzero]

Fair play for devising something that suits your situation, and works. Particularly the FB precipitation from water, that's a less-seen procedure.

 

[Jees]

The new approach was direct filtering...

You mean step 4 of your menu I presume. Well that's not a new approach either, it's described here at nexus in a few places. You must have found inspiration somewhere? Not many people do that style actually. Did such an experiment with ammonia once:

Backsalted liquid crashing out. No pull needed. - Collaborative Research Project - Welcome to the DMT-Nexus

^^^ that was done after a zinc treatment, so you have it simpler with no issues to avoid precipitating zinc-salts.

Also see step 7 of this post:

Discussing Alternative Spice Extraction Techniques - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

He said sticky and waxy, that is strange as I got mine very dry by using sodium carbonate.

Cool that you try out a non beaten path :thumb_up:

 

[GreenDMT]

Thank you Jees for finding similar posts. I understand that nothing is new, just I didn't saw this before. I have some knowledge of chem-bio so I tried to adapt somehow. Thank you for pointing links for similar treatment