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nen888
#101 Posted : 9/30/2013 2:58:47 AM
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DreaMTripper wrote:
a.floribunda phyllode tek

An acid simmer with vinegar was done x3, 45mins each. pH 5 solution.
Filtered then combined and simmered to 5-600ml
Based with lye to pH 12-14
Left to react
75ml of toluene added , jar shook up and left to settle, table salt used to clean emulsion.
np decanted off
Salted with roughly 30ml of pH 5 water/acetic acid solution
Np decanted and returned to main jar
vinegar/alkaloid solution evapped to 25ml
Poured into glass baking dish and sodium carbonate added , pH 11-12 reached.
Paste mixed up thoroughly. Took on a lovely indolic smell.
Dried on oil heater and crushed up with a knife and the bottom of a glass.
Put in tumbler and acetone added. Acetone pipetted away.
To be evaporated. Fingers crossed.


..thanks for the report DreaMTripper..good experimentation ..i don't know if the stage with 30ml acetic acid/water is neccessary..could leave more potential to lose a bit..
 

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DreaMTripper
#102 Posted : 9/30/2013 3:14:06 AM

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Thanks for the feedback nen.


End result was a small goo/stain, 30mg max.

Second toluene was separated and dried on oil heater.
Result: yellow honey oil with a brown blob of similar colour to previous acetone extract.
Again lit on a pin to test smell and again it melted with a nice pungent indole aroma.
 
DreaMTripper
#103 Posted : 10/1/2013 4:56:01 AM

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Now im guessing maybe the dmt has been oxidised from the heat to produce this yellowy brown wax or is this a combo of different alkaloids with plant oils mixed in due to no defat?
Anyone produced yellow wax/oil from floribunda by evapping toluene? Would you say it was n-oxide after bioassay?
No NMT in floribunda is there?
 
acacian
#104 Posted : 10/1/2013 11:39:43 PM

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you'll only really get a wax/goo from toluene doubt its oxides... with solvents like toluene or xylene it usually just comes out waxy or oily ..if its mainly dmt then it will form circular crystal like patterns, but they become a wax when scraped up

i remember reading that there were reports of nmt in floribunda, though I'd also read elsehwere it was mainly dmt... i excitedly await your bioassay- i've gotten a lot of wierd goos from floribunda down in victoria, though only one it seems had dmt, and a second test was negative
 
DreaMTripper
#105 Posted : 10/2/2013 1:41:18 AM

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Unfortunately it was barely active [b]however the smoking device wasnt appropriate for goo.
[\b]
No trippiness just a slight stimulation. Goo (or more like honeyoil hash)smells exactly like dmt but tastes of plant matter. Sticks to EVERYTHING! lol
Im guessing, just from reading, that its some dmt n-oxide spread throughout the plant oils, it melted at the slightest touch.of flame so I guess anything mixed in will have been ignited rapidly.

I also read the acacia analysis thread and noticed NMT had been found in floribunda so could explain the yellow tinge to the extract.

Thanks to the tree for providing the experience and practice and of course the extract.
Lessons learned.
Dont leave NP in mix for too long.
Dont leave base mix to sit for long.
Defat at after acid cook

oil and a blob of clear oil, dissolved whatever could of it in vinegarwater ; only the clear blob would dissolve. The amber oil is clearly just a 'plant oil' of some sort. Oh and it doesnt freeze.
Based then pulled again, evapped then dissolved in acetone and evapped on a bit of blue lotus.
Smoked in a well made spliff with weed and tobacco.
Slight stimulation again, Ozrics sound even better than usual but that could just be the lotus and weed. Likely so.



Note 2: was a commercial type bush rather than a tree.

Thats all folks..




 
DreaMTripper
#106 Posted : 11/14/2013 10:36:12 AM

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Phyllode tek expt 3.1 ( Based on nens phyllode expt 3)

a.longifolia phyllodes will report back observations, so far almost 3l plus of liquid used in de-gumming stage. Concerns the alkaloids have been extracted from plant matter during ethanol boil meaning long and tedious liquid reduction..
liquid is greenybrown.
strained plant matter in vinegar soak.
 
DreaMTripper
#107 Posted : 11/15/2013 1:11:57 PM

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No vinegar used in one, reduction by constant boiling over an hour was carried out on majority of liquid and strained through t-shirts.
Other liquid (from plant matter reacid boil) was reduced to 250ml with heat, based to pH13 and np (z#ppo prem) added.
Both resulted in dark brown tea like consistency.
Once lye solution was added a white cloud appeared at the top.
NP to be left over night and decanted sometime tomorrow evening.
 
DreaMTripper
#108 Posted : 11/15/2013 8:31:34 PM

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After being left to settle over night in basic solution 3 layers formed one green sediment on bottom third one amber in the mid third and one NP at top. NP (z#ppo pr*m lighter fl@#d) separated and left outside to reduce.
 
nen888
#109 Posted : 11/15/2013 11:00:55 PM
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..thank you for your observations DreamTripper..

i would not discard the alcohol solution..experiment 3 however suggested acidified water was a better medium for phyllodes..

it's an experiment though, not a 'tek'...

ultimately it's about finding the right ratio for what one wants to be soluble..
 
DreaMTripper
#110 Posted : 11/15/2013 11:58:54 PM

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Noted Smile Is there a possibility the alks couldve been filtered out of the solution when in the no vinegar alpha solutilon (pH6) ?
 
DreaMTripper
#111 Posted : 11/17/2013 1:00:17 PM

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In total 400ish ml of np was used to pull the tiny white crystaline substance and what was apparent was that the np was not efficient in dissolving it however when warmed did pull the white precipitate to the glassy surface of the red base layer to be picked up with a little base water, Precipitation in the np was occuring at room temp.
The solution is now a deep red and will be exhausted with toluene.
The story continues..



 
DreaMTripper
#112 Posted : 11/18/2013 9:52:02 AM

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Toluene was added and left to settle while the naptha jar was decanted into 4 tumblers and left for the cool night air to hopefuly form precipitates. Hope is that there is another hot day to evap as this is a long story.
75ml of Toluene pulled an interesting sandy brown powder to the basic mix surface. Uncertainty is whether the toluene is saturated or if it is insoluble in toluene. Same effect as naptha but more so and a different colour, hope is that this is the full spectrum. The base mix has stayed a dark red.
 
acacian
#113 Posted : 11/18/2013 10:56:22 PM

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nen, why would you say the acid wash reduces alkaloids? in my experience the yield has always been the same before and after - I think maybe with acacia it is better to not do it with straight vinegar but a ph 5 solution seems pretty reasonable to me... its a good way to rid extracts of unwanted impurities
 
acacian
#114 Posted : 11/18/2013 11:20:50 PM

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^^ yeah i've wondered what the sandy brown substance is that surfaces after basification... i often see it forming after leaving the basic mixture for long amounts of time. it doesn't seem soluble in np so I don't think its due to saturation.. toluene can hold a lot
 
DreaMTripper
#115 Posted : 11/19/2013 1:31:30 AM

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Yeah so has been noticed its cllose to saturation its very cloudy. What colour extract does toluene generally pull from acacia?

Zippo holds very little even when warm. Will see what happens when it evaps to freeze precip point as there seemed to be a lot in suspension but also couldve been a waste of time and money judging by the cloudiness of the toluene.
 
acacian
#116 Posted : 11/19/2013 2:19:11 AM

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depends on the acacia and the ratio of alkaloids (and type of alkaloids) to other compounds... most trees i've been testing lately have had yellow extracts.. and the ones that contain DMT smell very little like purer spice extracts. I guess the smell of an extract can vary a lot due to which chemicals its been in contact with its whole life- as every tree is differen't
 
DreaMTripper
#117 Posted : 11/19/2013 7:23:06 AM

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So ive been sent a pic of the surface mystery sandy stuff, appears much surfaced overnight..
Zippo didnt pull this only toluenevl however zippo pulled similar composition but it was white..This could be a real cosmic joke if none of this is active
.Answers on a postcard..
Some of this was separated and left to dry inevitably basemix was pulled also so a clean up is needed once dry but it looks of a crystaline structure. What colour is harmala/harmine freebase?
Its of a similar colour to the google pictures..
DreaMTripper attached the following image(s):
IMG_20131119_183402.jpg (231kb) downloaded 551 time(s).
 
DreaMTripper
#118 Posted : 11/19/2013 9:03:27 PM

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Ive been told it dried to reveal a tan crystaline pattern so will be cleaned with basic cold water..
Supposedly smells like almonds, as it happens smells like an a.verticallata that was encountered and tested that yielded a similar extract maybe THAT tree was packed full of this substance and the extract just needed washing..live n learn
..
Substance twinkles but doesnt melt and burns to a cinder so may well be the lye/plant water contaminant doing this.
First pull was much lighter in colour than the first and it appears there is a lot of this subtance in there..
Meanwhile in the zippo tumblers (going through a night and day cool then evap cycle) there are bright white crystaline flakes floating and resting on the bottom, hope is for another few hot days so freeze precip can be done and the substance looked at closer.
Extract maybe 1-1.5g so far not including the zippo pulls however no chickens are being counted could well be another acacia red herring, who is it that is realy getting tested here?
Must also be noted that despite the dark red colour of the basic mix nothing of that colour has been pulled is there still an alkaloid in there that is neither soluble in toluene or light naptha?

Update: dirty crystals were put in a tumbler of salty saturated Na2CO3 to precipate and lose the gunk, immediately white floaties could be seen in the orange liquid. So back to the naptha tumblers tomorow evening... the saga continues..

Update: water crystallization has failed, many white microscopic flakes could be seen in the orangey basic water yet a tiny amount of white flakes were sitting at the bottom.
From nearly a gram to almost nothing..Will update how the naptha evap cycle is going..
 
DreaMTripper
#119 Posted : 11/23/2013 1:27:23 AM

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Well this is incredible. Solution washed new solvent (toluene) added and evapped and Im told it looks very clean now waiting to dry.
Speculation is to get everything out a litre of toluene would probably be needed as it just keeps coming. Amazing.

In the original alcohol extract jar toluene was left for a week and it saturated and pulled brown powdery clumps to the top.
The floaters were specifically targetted and separated and washed.
In the washing jar the powder is lighter now and will need another cleaning. In the solution underneath the surface can be seen offwhite precipitate. So its fairly soluble in toluene, slightly soluble in basic salty water.
Starting material was roughly 300-500g of phyllodes and twigs.
NO INSECTS SEEN. Red tips. Leathery thick dark green phyllodes. Very robust and waterproof.

 
acacian
#120 Posted : 11/23/2013 1:57:50 AM

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look forward to hearing results... I am wondering at the moment whether maybe in some trees there are certain compounds that trap the alkaloids making it hard for a single solvent wash to pull em all out.. a single pull with toluene should be getting it all out, but i just did another pull on this longifolia extract and pulled out just as much as I did off the first one. will bioassay it in a bit to see if it is as high in alkaloid content as the first pull
 
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