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Sulfites to help break up lignin while basing? Options
 
Loveall
Chemical expertSenior Member
#1 Posted : 9/18/2019 3:34:53 AM
Attaching a paper claiming that sulfites can help break up lignin (the material that gives plant cells toughness). See image bellow where there appears to be more openings for extraction when using sulfites with NaOH instead of NaOH alone.

This could help in extractions. As a gross check, I added potassium metabisulfite to some "spent" STB bark. Calling it "spent" after 5x naphta pulls with minimal xtals in the last pull. Ran the "spent" bark with sulfites added through the pressure cooker. Pulling after that (t
he 6th naphta pull) I got xtals. I can't say for sure if it was the PC run that did this though (instead of the sulfites).

I'll do more tests to see if there is anything to do this. I'll simply add sulfite salts (10-20% is my guess) right after basing. These salts are cheap and easy to get. For example, there is a product by bonide called "Stump-Out" that sells for $7/lb and is sodium metabisulfite. It is marketed to remove tree stumps chemically as you might guess.

A good way to check if sulfites can help with DMT extraction from bark would be a split experiment where the control has plain salt added to keep the same ionic strength (moles of salt) as the sulfite condition.

One caution is to avoid sulfites in acid. While lignin is also attacked in this situation by sulfites, toxic SO2 will be released in acidic PH and your house may smell like a stinky paper mill.
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downwardsfromzero
ModeratorChemical expert
#2 Posted : 9/18/2019 11:25:29 PM
SO2 is particularly bad for asthmatics. That's a really important reason not to add acid to sulfites.


Note that the sulfite treatment (as detailed in the diagram you attached) takes place at 140°C. That's considerably hotter than your usual pressure cooker.

It's reasonable to suggest that PC treatment, the sulfite and simply the passage of time will all have contributed to releasing that final yield of crystals. As an informed guess, I'd say that some of the tannins will have been broken down as well and possibly some oxidised form of the alkaloid will have been reduced too.

I love how you keep on trying these interesting experimental methods - keep up the good work! Love




“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
 
Loveall
Chemical expertSenior Member
#3 Posted : 9/19/2019 2:20:57 AM
Yes, you are right DFZ - my PC runs at 15 PSI which means it gets up to only 121C I believe (I live at low altitude).

I'll report back in a few weeks. It could very well be that the sulfites don't help in the kitchen, let's see what we get.
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Loveall
Chemical expertSenior Member
#4 Posted : 10/1/2019 6:49:11 AM
Ok, so I did a STB where I added potasium metabisulfite from the local brew store. I used a 1:6 shredded MHRH bark to water ratio mentioned in the paper in the first post (50g of bark and 300ml of water) then slowly added ~10% NaOH (30g) and 20% (60g) Potasium Sulfite. This was mixed well and run in the PC for two hours at 15 PSI, then allowed to cool below 100F and pulled 3x with naphta.

Notes/Results

- Part of the bark turned into a thick muddy slush and a distinct "pulp" like core. Seems consistent with the lignin breakup to release the cellulose story, but I can't say for sure.
- During the naphta pulls a burnt tan/orange color appeared in the naphta (see first image below). Usually with NaOH only looks more yellow.
- This orange color is difficult to get rid of. It remained after a few re-X (it only slowly fades). It is a bit problematic honestly (assuming it is unwanted). Right now this is a downside compared to doing STB with NaOH only (from previous experience).
- On the plus side, yield was surprisingly high after only 3 pulls (1.008g ~ 2%, however the product is now white yet - see second picture). I usually get less with a simple STB after 3 pulls (1.5% to 1% range). Will do a few more pulls to see if anything else comes out.

So sulfites could be helping break up the bark?

Overall I think this is worth a few more tests. If we find a way around the new orange color (e.g. a FASA/I step) it would be worth doing the direct sulfite/no-sulfite split keeping all else the same (same PC run, same ionic strength using NaCl on the control) to compare yields.

Also, I may have overdone it. It could be that with sulfites less NaOH is needed, etc. But first, will need to figure out the orange color and then check yields. If no benefit at that point it would not be worth fine tuning this process.
Loveall attached the following image(s):
IMG_20190925_074315751.jpg (3,027kb) downloaded 101 time(s).
IMG_20191001_011530967.jpg (2,042kb) downloaded 100 time(s).
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leratiomyces
#5 Posted : 10/1/2019 10:20:17 AM
Tried a quick acid base extraction to see if the colour remains in the organic phase?
 
Loveall
Chemical expertSenior Member
#6 Posted : 10/1/2019 12:47:48 PM
No, haven't tried a mini A/B for cleanup. Good suggestion, thanks.
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Loveall
Chemical expertSenior Member
#7 Posted : 11/17/2019 10:49:01 PM
leratiomyces wrote:
Tried a quick acid base extraction to see if the colour remains in the organic phase?


Done.

After the STB with the sulfites as described above and and a naphta pull, I did an A/B on the naphta. It was neat to see the naphta could up during the A, and hem the water clouded up during the B.

The red color is essentially gone and an off white fluffy spice results. Good stuff. Yield was 1.3% and I know I can get a little more with more pulls. Based on my previous experience with the bark material this is a very respectable yield.

So sulfites may be worth a shot for those who like STB to help dissolve lignin and release DMT, but a mini A/B may be needed after. The final A/B is easy to handle since thighs are relatively pure and the clouding is a good indicator of what is happening.

Using sulfites may allow using less NaOH and still have an effective extraction. May be worth testing one day for a less caustic profess that can still penetrate the bark.

Cheers.
Loveall attached the following image(s):
IMG_20191117_173155002.jpg (3,334kb) downloaded 70 time(s).
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Tony6Strings
#8 Posted : 11/18/2019 6:30:45 AM
Very cool. Did you smoalk any of the orange stuff before re-x? I've pulled orange-ish red-ish spice that was fantastic, STB with naphtha (mine went dark like yours). Hey is that an AWS Gemini 20? I've got the same scale and I love it!!
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Loveall
Chemical expertSenior Member
#9 Posted : 11/18/2019 11:24:40 AM
Yeah, smoked the redder stuff and it and it was fine Big grin

And yes, that's the same scale. Good stuff.
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Loveall
Chemical expertSenior Member
#10 Posted : 12/7/2021 3:13:43 PM
Looking back at this, I believe the red color was from partial DMT polymerization in the unusually high ionic strength STB.

Can't say for sure though. Main data point is that it vaporized fine with good effects without leaving residue behind 🙂

I now think more dilute TEKs with gentler ionic strength minimize DMT polymerization and give better results (e.g. max ion). Bark breakdown does not seem to be a yield limiting factor.
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Dirty T
#11 Posted : 12/7/2021 6:32:51 PM
I always get red amd brown DMT on end pulls and it's always been fine. The difference between it and white DMT is not noticeable. The only difference as far as I can tell is color and texture. 15mg white and 15mg red/brown both give me the exact same effect and 30mg either is a breakthrough dose for me.
 
Loveall
Chemical expertSenior Member
#12 Posted : 12/7/2021 8:39:42 PM
Dirty T wrote:
I always get red amd brown DMT on end pulls and it's always been fine. The difference between it and white DMT is not noticeable. The only difference as far as I can tell is color and texture. 15mg white and 15mg red/brown both give me the exact same effect and 30mg either is a breakthrough dose for me.


Same here. I only notice a difference when fine tuning electronic devices and setting the temperature low for the smoothest/coolest smoke possible. White xtals vaporize at the lower temp.

I imagine if complexing with | High Pobability of Braindamage by Creepy non tested Drugs (forced by scammer 69ron) | one wants less aggregation, but I don't have experience with that.
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