Low yield due to formation of Dmt Oxide?

[omnilucident]

Some of you are probably starting to notice my never-ending trail of pleas for help on these forums.
after many many extractions using acuminata phyllodes, and my recent two attempts with bark I have never been able to surpass a 0.05-0.1% yield.
I have adapted many many changes to my recipe and while I have had improvements, I have not broken through into anything like what everyone else on this site seems to get.

I recently had an idea and would like other's input.
up until very recently I did not realise the signifigance of low heat in an extraction. I had always the thought that because shellite's ability to hold dmt increased with heat, that using heat baths of boiling water and adding excess lye throughout would be positive for my yield.
But recently I discovered that dmt+heat+oxygen creates dmt oxide (correct me if this is oversimplified).
So what if the fact that my basic soup had boiled and been shaken a lot before any solvent had touched it (plus lots of heat and oxygen shaking after solvent added) meant that most of the dmt had already converted and thus was not soluble in shellite/naphtha? (read somewhere that dmt oxide was insoluble in naptha)

another reason for me thinking this is that I have never gotten anything remotely like white crystals from freeze precipitation, only small amounts of bright yellow crystals and large amounts of oil frozen to the bottom of vessels (which is re crystalised).

I personally prefer the white n-dmt but have a lot of difficult acquiring it.
the only time this system was good for me is when somehow I managed to precipitate dark green crystals from the phyllodes of acuminata. I strongly believe that the green tint was from plant oils that contained an MAOI (hyperspatial visit was noticably longer) and other interesting compounds. After a session last year with several friends we all agreed that the green crystals contained a friendlier and more helpful spirit than any other we had encountered with dmt.

anyway, sorry for such a long post but I thought this might trigger an interesting discussion.

 

[DreaMTripper]

Still no luck, bummer..shellites a terrible solvent to use (as are most Aus naptha it seems from reports) that could be THE problem. What else do you have available there?
Have you read this thread? A ratio for acuminata is included in the second post just swap DCM for xylene or toluene.
The Acacia Analysis Thread - Plant Analysis and Substance Testing - Welcome to the DMT-Nexus

An idea maybe to tweak cybs salt a-b tek but before you do soak the phyllodes in just methylated spirits for a day and shake often then filter the liquid and keep it aside for extracting anything pulled into it after.
Then soak the phyllodes/powdered bark in vinegar water and freeze it to lyse the cells. Thaw it out and then follow cybs tek here Cybs' Hybrid ATB 'Salt' Tek - DMT-Nexus Wiki but use toluene or xylene instead of naptha and evaporate. You could then reX in a widely available heptane glue remover or z$pp@ lighter fluid.
I recommend that tek as its primarily a one pot tek that will reduce loss as there is no multiple container transfers.
Any A/B tek would probably work a long as the plant material is thoroughly lysed and pulled with a suitable solvent, the metho wash is there to separate the gums that have been seen to obstruct extraction.

 

[omnilucident]

Boiling methylated spirits sounds ridiculously dangerous, how would one do that with low risk. and would I just mix that metho with acidified water later to recover any desired alkaloids?

I had actually freezed and thawed bark in the past but I never had soaked it in acidified solution, they were just dry :/. thank you very much, I will definately do that next.

as for that tek, I haven't heard of anyone doing STB with Acuminata so I assumed it wasn't very efficient. I did add something like 3-400grams of salt (contained an anti-caking agent) to the 2kg soup.

also, has anyone actually found easily accessible heptane in australia?

I'm currently trying a pull of 500ml xylene on the 2kg soup and will try to mix the xylene with acidified water (5x200ml pulls) then basify and pull with zippo fluid. does that sound right?

thankyou so much DreaMTripper, I feel hopeful yet again.

also if anyone sees this who works with acuminata know whether they have started developing flowers yet? I want to collect some phyllodes but don't want to drive out if they have lost their yield for the time being.

ultimately if I can crack this extraction, I pledge to create a pictorial trek for a sustainable (foodsafe/salting/recycling solvent trek) for using the leaves of the acuminata.
maybe it will be deter some of the countless young people from ring barking trees all over w.a. in some areas it is becoming quite horrific.

 

[DreaMTripper]

Thats terrible but sadly not surprising I hope they get a harsh lesson in hyperspace and maybe some will see the error of their ways..

The boiling in methylated spirits is not advisable in a layman kitchen set up to be honest a long cold soak is better and much safer or at least use a water bath set-up.

Yes you can add acidified water or just basified water to the filtered solution after. Then pull as normal with a NPS. ( The heptane you ask about is in the 'solvents in australia' thread have a read. )
Experiments have shown that there wont be much alkaloids pulled in that solution but there will be obstructive gum.

You should do the acid step in cybs tek if you do follow it as STB isnt recommended for Aus acacias.

I'm currently trying a pull of 500ml xylene on the 2kg soup and will try to mix the xylene with acidified water (5x200ml pulls) then basify and pull with zippo fluid. does that sound right?

thankyou so much DreaMTripper, I feel hopeful yet again.

Let me get this straight are you going to pull on a basified mix with xylene? Then add vinegar and water to convert the dmt back to salt form? Then re-basify and pull with lighter fluid? It will need to be hot solvent so its saturated to enable succesful freeze precip later.
Sounds a good way to concentrate the spice let us know the result!

There seems from what ive read to be some key points that have to be completed fully for a successful extraction a) thorough lysing b) solution is in the right pH range at the right stage c) amount of solvent and type of solvent used is sufficient for the size of the solution and the type of alkaloid being targetted.
d) when reX the solvent MUST be supersaturated to precipitate the maximum spice..
Have a think if you have adhered to these.

 

[omnilucident]

i mean is it safe to boil in regards to flammability. you're saying put the phyllode powder in pure methylated spirits and boil? I only have a gas stove but perhaps I could purchase a portable hot plate.

that is correct, that's my plan.

see with diggers shellite it seemed everything would freeze out regardless of how saturated it was. but using naptha (z#ppo) changes that a lot. I have some old used solvents (shellite and z@pop) that I thought were empty, perhaps if evaporate them down to 1/5th of size and freeze them, I might get something I didn't know was in there.

are ph papers considered accurate enough for ph testing? I know my solutions are always basic enough as I use more lye than I possibly need to be sure as ph papers do a shitty job with barky solution. but perhaps the acidic stage isn't as accurate as I thought. is there any harm in going to a ph of 3 instead of 4 or will that have a negative effect on yield?

 

[DreaMTripper]

Edit: In a layman set-up as most have it is unsafe and inadvisable to boil such a flamable liquid such as methylated spirits (95% ethanol 5% water)
Shellite may freeze precip easy but you have to get it in there in the first place to a saturated level..the general rule is to reduce until it clouds when you blow on it

You should definitely reduce those old pulls as you may get a nice surprise!

pH papers are good to use.

 

[downwardsfromzero]

It is not safe to boil any flammable liquid in an open pan over an open flame.

The water content ensures it isnt that flammable. [...]
you may get a nice surprise! [for actual context of this last phrase, original quote is in post directly above]

Or a nasty one. I would suggest you edit your advice about heating flammable solvents, DreaMTripper.

I would suggest using a waterbath. And possibly a lid.

SAFETY

 

[Du57mi73]

A long time ago i would store all my freeze precip naptha after every freeze. i reduced 2L down to 500ml, then I froze that. I got another 5g. Worth it.

Also, the formation of n-oxide is alot less common that speculated to be.

 

[DreaMTripper]

It is not safe to boil any flammable liquid in an open pan over an open flame.

I would suggest using a waterbath. And possibly a lid.

SAFETY

You are correct it is not safe to boil any flammable liquids on an open flame a prolonged soak in a waterbath would be as effective and much safer. I also suggest you edit my quote into the context it was originally written in.

 

[omnilucident]

yeah, as a recovered pyromaniac I wasnt actually going to boil metho on a gas stove pot.
how long would I need to soak to have a similar effect to 30 minutes boiling?

thanks for all your help DreaMTripper!

 

[DreaMTripper]

No worries man I wouldnt like to see any harvested material wasted its just the plant testing your resolve to see if youre worth its gifts

1)A large jar with the phyllodes completely submerged in metho but only a tad above the plant layer. Rigorously shake it with lid on tight.
2)Boil a pan of water take it off the stove put the phyllode jar in and unscrew the lid to allow any pressure to release.
3)Leave in waterbath until its cooled then remove and let stand for an hour or so
Screw lid on tight again and shake vigorously.
Repeat over a 2 day period then drain off the tarry liquid.
The phyllodes will then be nice and shiny with the gums and tars removed.
4)Cover the phyllodes in vinegar water, one cap of 5%vinegar/litre.
Place in the freezer overnight then take it out and let it thaw to room temp. Do another freeze thaw if you like but it probably wont be neccessary now.
5)Now either follow the BLAB tek or cybs acid to base hybrid tek keeping phyllodes in or you could simply boil 3x for 45 minutes drain liquid and replace with new.
6)Then filter out phyllodes and combine the 3 liquids and reduce to 750ml. Put liquid in a bottle or jar. Rigorously Defat with shellite not xylene. remove shellite.
7)Basify , add salt, let stand to react.
Pull with 100ml of xylene 3 times.
Evap the xylene to leave full spec extract.


That encompasses pretty much all Ive read about phyllode extraction and recent teks and adheres to all the key principles of extraction and is adapted to PHYLLODE extraction. If no yeild after that then youve ID'd wrong or havent followed it properly.
For bark remove the metho soak step and just freeze thaw a few times in vinegar water. Now all I need is to move to WA and try it myself!

 

[Du57mi73]

No worries man I wouldnt like to see any harvested material wasted its just the plant testing your resolve to see if youre worth its gifts

1)A large jar with the phyllodes completely submerged in metho but only a tad above the plant layer. Rigorously shake it with lid on tight.
2)Boil a pan of water take it off the stove put the phyllode jar in and unscrew the lid to allow any pressure to release.
3)Leave in waterbath until its cooled then remove and let stand for an hour or so
Screw lid on tight again and shake vigorously.
Repeat over a 2 day period then drain off the tarry liquid.
The phyllodes will then be nice and shiny with the gums and tars removed.
4)Cover the phyllodes in vinegar water, one cap of 5%vinegar/litre.
Place in the freezer overnight then take it out and let it thaw to room temp. Do another freeze thaw if you like but it probably wont be neccessary now.
5)Now either follow the BLAB tek or cybs acid to base hybrid tek keeping phyllodes in or you could simply boil 3x for 45 minutes drain liquid and replace with new.
6)Then filter out phyllodes and combine the 3 liquids and reduce to 750ml. Put liquid in a bottle or jar. Rigorously Defat with shellite not xylene. remove shellite.
7)Basify , add salt, let stand to react.
Pull with 100ml of xylene 3 times.
Evap the xylene to leave full spec extract.


That encompasses pretty much all Ive read about phyllode extraction and recent teks and adheres to all the key principles of extraction and is adapted to PHYLLODE extraction. If no yeild after that then youve ID'd wrong or havent followed it properly.
For bark remove the metho soak step and just freeze thaw a few times in vinegar water. Now all I need is to move to WA and try it myself!

That was extremely informative.

Why do you suggest defatting with shellite and not xylene?

Also, what requires the need to move to WA? That sounds like it can be done anywhere. haha

 

[DreaMTripper]

Its where the acuminata are , for me importing acrb into Australia is way too risky. So I read until I find an other option.
I said to not use xylene as its an aromatic solvent and someone mentioned the salt form of dmt is slightly soluble in it, how true that is I dont know..learnt most of that method just from reading the acacia workspace thread.

 

[downwardsfromzero]

[...]
I said to not use xylene as its an aromatic solvent and someone mentioned the salt form of dmt is slightly soluble in it,[...]

I was reading only the other day that it is the acetate that has noticeable solubility in xylene. The fumarate is more polar so there is much less of a xylene solubility issue. Don't remember which thread either.

 

[denyr1]

I have no problem getting roughly 2 grams from 100g of acuminata using a simple stb tek. It may not be pure clear crystal but I am sure a wash would fix this. I haven't advanced that far yet unless I have an excess amount of spice to practice with.