Same plant different outcome

[Tryptallmine]

Ok, so there is a what Is beleived to be an A.Floribunda or longfolia so a clipping of 25g eyed it was taken, before realiseing there was about 3kg of bark that had come off the plant naturally so enough for a small run was collected

After a couple of extractions, Cyb's Salt tech, no freeze thaw etc. Basically just got it fibrous both bark and the other phollodes/twigs/flower spikes.

Acid Stages (ph2), Basified stages (Ph 12)

Set 1. Phollodes etc, seemed to go ok, the usual yellowing on the NPS pulls x 4. didn't yield a geat deal, clouded up which would indicate it was adequately saturated, leaving that one in the freezer but shows promise.

Set 2. Bark (not root but close enough to the base of the tree). Over compensated on the bark and used 65gm instead of 50.

Heres what is not understood, the bark was nice and thick and obviously not 'live on the tree' and no one wants to start hacking into a tree.

The same process was conducted as before however the result contained an emulsion in which a little more NaOH was added to try and remove it - didn't exactly happen. With some success a little was removed with a baster.

Anyway. The warm pulls were done @ 70 deg naptha on room temperature base solution. Mixed end over end and allowed to separate 4 times in a 50-55deg heat bath only to pull very clear solvent back out of the soup. Rinse and repeat....

Not even the slightest hint of yellow. It was as if it was returning straight naptha back out? When it was reduced/evaporated to a lower quantity of liquid it it did turn milky but not as saturated as one would expect.

It appears as if there are some minute crystals forming but it just doesn't seem right that it came back so clear?

The morning will tell the truth, but if any of you have some thoughts it'd be a great help.

Cheers,
Trypt.

 

[DreaMTripper]

Acacia floribunda and longifolia have varying alkaloid profiles throughout the plant and throughout the year.
Apparently sometimes they have no psychoactive alkaloids, sometimes a ratio of NMT and DMT and betacarbolines, which also varies.
Acacia generally need good lysing too.

 

[Tryptallmine]

I suspect a misidentified species. Maybe a tiny clipping off the tree over the next day for an ID. In hindsight it looks more like a coastal wattle however its far too inland. Same phollode profile.

The other thing considered in thought, was the that when NPS was added there wasn't the usual production of gasses/fizzing you'd expect and that had been noticed in other extractions. What would be the cause of that? - like a positively identified A.Floribunda or A.Maidenii.

The soup hasn't been discarded yet, it sat overnight so maybe a slight reheat and attempt another pull to see if time was the issue. The acid soak was for 1.5 hours and basified for about 2 before pulls. All it around 50-55 degree celcius heat baths.

Probably much of the colour from the first run is the result of chlorophyll and plant oils. After a quick sodium carbonate rinse a bit of that colouring came out however yielded pretty much nothing, was mildly active with the 10mg or so that was collected.

The clear liquid dropped a few cystals out even when cooling to room temperature on the bench but just specks.

Any tips on getting rid of that 2mm emulsion layer? Syphoning off some and adding more NaOH didn't really work.


***Maybe a little too hasty in the conclusion process*** look ok?

Was thinking that it might just disolve back to solvent. It's upside down on paper in a freezer right now draining off residual naptha.

 

[Tryptallmine]

And it dried to nothing and disolved back to a liquid. Blow on it and it clouds up again?
There is some distinct confusion here.

A lot of research but why does it always melt back to solvent?
Not a high enough saturation? It seems quite cloudy albiet white.

Pulls were combined into a dish and evaped with a van to form the cloudy liquid.

There is another pull gone in with a lower freezer temperature, it'll see a longer duration in a freezer. It seems that moisture seeps in despite covering in gladwrap and then sealing the lid on tight.

Or is the trick to drain off the solvent and keep freezing it?

Most extractions bar 1 have all ended up the same way.

The indifferent extraction came back to some slight crystals and some very active goo to the sum of around 700mg from 54g of bark obtained from a snapped branch after a storm of A.Floribuna. So it was quite fresh.

 

[DreaMTripper]

700mg of actives from 54g is a good yield! Explain further when this 2mm emulsion happened..

 

[Tryptallmine]

700mg of actives from 54g is a good yield! Explain further when this 2mm emulsion happened..

Thanks for chiming in DreaMTripper, appreciated.

There was no complaints with the 700mg agreed, goo or crystals - it's all wonderful stuff.

Obtained a small clipping of the same A.Floribunda (confirmed) that previous actives were extracted from today, so another small 50gm extraction is on the cards when time permits.

Now to the emulsion. Greatly suspect it was a contamination of having not cleaned the glassware correctly. Usually glassware is rinsed for a while with tap water then run naptha or iso through and coat/swirl completely and let it evaporate. Seems to have worked in the past - any tips there are appreciated.

The emulsion formed after the cold base was added to the warm acidic solution and agitated. Previously mentioned the acid soak in a heat bath was at a pH of 2. 35gm NaCl and Deionized water combined and heated. Not all the NaCL would disolve so more deion H20 added until complete saturation then drew off the required amount of liquid and added it to the main vessel. 50gm of NaOH was added to the prescribed 200ml deionized water added to the mix then topped up with the extra 140ml. It wasn't quite dark enough and the pH was a little low around 10.6, so 10gm more was added which raised it to 12.4.

The vessel was agitated lightly and rolled end over end, swirled to prevent settling and a good mixing motion. The emulsion starts to present itself here. More like a spotty / patchy layer of something. The same type of something that if you were to pull some basified solution and place it on clean glasswear and allow to dry, that colour, texture and symmetry.

A tiny bit more NaOH was added again to try and remove the emulsion. Then tried to syphon it off. More kept forming with each agitation - maybe trace amounts of detergent. But always the same sized layer. After the second heat bath it was quite established - the emulsion that is. Heat baths were kept around 50-55 degrees monitored with a thermometer.

What do you think of both the pictures? Saturated enough?

It looked quite clean in the post precipitation picture but it is as if it is some type of crystalisation that disolves back to water/solvent. It has to be some extraction of matter, water doesn't freeze like that, and we know naptha and ethanols don't freeze.

The combined pull in the first picture has been in the freezer now for 24 hours, it will remain there for a further 24 hours in the interest of patience and its importance in the process.

A hairdryer (cold air) was used blowing freezing air from the freezer into the dish to evap off the naptha after having left it sit upside down on paper for an hour. Then it all turned back to liquid.

With a bit of luck this serves you enough information. :thumb_up:

 

[DreaMTripper]

Dish 2 looks saturated enough, dish 1 not so much by that pic.
Definitely worth the small effort to back-salt and rebase to further separate the alkaloids from any non-actives.
Then you should be able to pull with less NPS in one or two warm pulls. Or with room temp toluene/xylene if youre after as full spec as possible.

 

[Tryptallmine]

Dish 2 looks saturated enough, dish 1 not so much by that pic.
Definitely worth the small effort to back-salt and rebase to further separate the alkaloids from any non-actives.
Then you should be able to pull with less NPS in one or two warm pulls. Or with room temp toluene/xylene if youre after as full spec as possible.

Back salt and rebase...a bit lost now. Only managed a few extractions so forgive the lack of understanding.

If you could shed some light on what you mean it'd be appreciated.

Take it back to a salt by acidifying and then rebasing in a small volume and re pull?
Is that what you mean? a mini A/B so to speak?

Again sorry for the confusion. It's a learning experience after all.

Dish 1 hadn't been in the freezer yet, dish 2 was post precip. Might get reduced some more. Thanks

 

[DreaMTripper]

Thats exactly what I meant

Do you have a good detailed pic of the plant? Also the state it was found in and wether its a coastal or inland area ?

 

[Tryptallmine]

Will grab a few snaps tomorrow. It's inland 80 odd km. Suburbia.

Having looked at the trusty Native trees and Shrubs of South East Aus book, there would be bets placed on the plant being A.longifolia var. sophorae due to the rounded nature of the phyllodes and relatively short length. Probably should have consulted the bible first. The shrub in question has such dense spikes in terms of numbers.

I think defeat is about with this particular sp. The sealed container has evaporated all the naptha over a 30 hour period....seriously odd.

Seems to be mostly ice and cloudy white crap, may try a mini A/B in the morning but i think the tried and true A.Florabunda might be a little more worthy of the time.

So below are pics of the A.longifolia var. sophorae, followed by ye ole faithful A.Floribunda which yielded 700mg of goo from 54g previously.

 

[Tryptallmine]

ditched this post.

 

[Tryptallmine]

Is there a point either way where you can have the material in an acid soak or base for too long?

3/4 of the way through a run with 100gm of bark and decided to take some time time with it. Prepped the bark into very fine powder mixed it up with the de-io water and froze it until hard, thawed it, twice. It had an acid soak in heated cycles warm to room temp for about 3-4 hours then it was left over night wrapped in insulation to keep it from getting to cold.

Mixed it all up this morning and put it back on the bath, added NaCL to the soup and based. T+3 hours in its going through its second heat/cool phase. Need to leave it there for today and cant continue. Will have uninterrupted time tomorrow to pull the mix.

Anyone see any issue why you can't just leave it sitting based for 24 hours and give it another heat cycle/mix in the AM?

--------------------

Figured where the previous mishaps were. Wasn't letting the NPS mix with the base soup long enough. Added one round of solvent for about 10 minutes and called that a pull. Then did 4 of those over 40 minutes rather than 1 pull mixes for 40 minutes then is removed. Repeating the process taking multiple hours.

Completed a tiny test run on the current soup last night on the side, based it mixed the NPS for 40 odd minutes for a single pull with 30ml of naptha. Sure enough the good stuff started falling out in ambient temps. Letting it cool to room temp-> fridge -> freezer was much better than straight freezing.

 

[DreaMTripper]

Looks like some nice juicy cuttings of flori you have there!
Nice red tips too I would be surprised if you dont get anything psychoactive from them.

 

[Tryptallmine]

0.87g after a re-x on the first two pulls. Fairly happy with that little florry, its a proven returner. Very very fine fluffy crystals and powder. Cleaned up well, around 30mg sent this black cat into hyperspace instantly.

Bit of water in the second batch pulls. Combined, evaporated down and pulled the water from the mix. Gone back into the fridge then freezer.

Bit of luck it returns around the same which would net a 1.5-1.6% yield. Even if it doesn't that's plenty of spice for a while. Processes are getting better every time but you'd expect not optimal from only a handful of extractions.

Pic to come.

 

[DreaMTripper]

Very nice! That was from phyllodes/stems and branch bark was it?
Looks like you have a good ally there look after it and Im sure it will look after you.

The a. sophorae may well have been a histamine type
More info about that here..
Trying to improve Acacia information - Collaborative Research Project - Welcome to the DMT-Nexus

 

[Tryptallmine]

Very nice! That was from phyllodes/stems and branch bark was it?
Looks like you have a good ally there look after it and Im sure it will look after you.

The a. sophorae may well have been a histamine type
More info about that here..
Trying to improve Acacia information - Collaborative Research Project - Welcome to the DMT-Nexus

That was from 110gm of branch bark and a few twigs - small clippings, not up for carving up a tree. There's still 250gm of phyllodes which could be interesting to try an extraction from. They are almost dried up as they've been sitting there for 2-3 weeks.

The other batch is looking alright, evaporated down to 30ml of naphtha. Nice structure starting to form in the bottom of the beaker. Very milky, cloudy white colour solution.
The first run was a touch more yellow in colour before the re-x.

The last time this plant was used was when the weather was a little warmer, around September and it returned a lot more yellow goo. Little less colour in the winter.

 

[DreaMTripper]

Good on yer mate good to see another tree friendly extraction success.