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Seldom
#41 Posted : 11/26/2012 8:06:12 AM

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interesting. thinking about comments here makes me wonder what's gone on with this extraction from a while ago. the tree is actually a. filicifolia. the little crystal seemed to crossover immediately on contact with the hot naptha, swirl around following petering out convection currents and eventually sink to rest and eventually dissolve on top of the polar later. i don't know enough chemistry but does anyone know if it would make sense that some alkaloids may be insoluble in naptha at both extremes of heat ?

polar layer was cool, and the naptha hot, the reduction of temperature in the naptha on initial contact with the polar may have let whatever it was quickly cross over, but the subsequent temperature increase in the np layer as the rest of the naptha was poured in brought it out of solution. maybe.. makes me think it's worth re-testing, roots were found dead and protruding from a river bed.
 

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nen888
#42 Posted : 12/2/2012 7:40:57 AM
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..thank you thick-light..good effort!..
as i wrote in your thread:
Quote:
..Jim de Korne who used naphtha Never heated his solvent, and got plenty of dmt out..

the concept of 'solubility' and NP solvents is more complex than discussed usually..
it is also a case of charge, meaning that the molecule is more attracted to the NP solvent, while not necessarily 'soluble' in the absolute sense..

NMT turns rapidly yellow over time..

DMT has usually been found to be the major alkaloid of A. confusa..


..i suggest a lot of people's 'problems' with acacia extraction may relate to heat..
a little may be ok..a lot not..

old-school naphtha lore used time (several days) , swirling and multiple pulls to achieve good and importantly efficient extraction results..i feel like the heat method may be an impatient adaptation that perhaps suits mimosa, but not many other plants..
 
thick-light
#43 Posted : 12/2/2012 8:20:57 AM

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Do you think the heat destroys alkaloids that may be active and interesting?

This was my last pull left in the freezer for 12 hours. It's pasty and started turning yellow pretty fast. It also has the same beige pasty color and consistency.
thick-light attached the following image(s):
last freeze for tonight.JPG (238kb) downloaded 1,479 time(s).
I love all of you!
 
nen888
#44 Posted : 12/4/2012 11:48:17 PM
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thick-light wrote:
Do you think the heat destroys alkaloids that may be active and interesting?

This was my last pull left in the freezer for 12 hours. It's pasty and started turning yellow pretty fast. It also has the same beige pasty color and consistency.

..i think excess heat can trap alkaloids with other components within the basic solution..or, at least let it cool down before draining the NP layer..that's my theory anyway..

btw, the 'multiple pH' suggestion was meant only for very thorough experimental work, or if one suspects there may still be alks in there..

..your process, results, and journaling of this extraction are great thick-light..especially for a first attempt!
the Force is with you!
i think it should be included as the Acacia Thick-Light Tek in the Nexus-Wiki..Smile

the 'beige pasty' putty has a good chance of being, say, three quarters dmt with some nmt and traces..
NMT (depending on how much is in there) will have continuing effects after the dmt effects have diminished..it can also slow down the onset of the 'flash' (especially with betacarbolines), which most (who've tried it) prefer to the severity of DMT on it's own..if a 'breakthrough' is required, 'just smoak moar'..Smile
.
 
nen888
#45 Posted : 12/9/2012 5:58:15 AM
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..the image attached below was provided by the person doing the experiment observed on p2 of entheogenic effects of nmt
Quote:
.the other month, however, i observed an experiment in which 100g of material known to contain dmt/nmt was extracted with ethanol/methanol/acetic acid>NaOH>dichloromethane..the solvent/alkaloid mix, when almost evaporated was placed unsealed in a freezer (to allow H20 condensation in order to 'skew' the re-x according to polarity)..upon removal the mixture had partitioned into white circular dmt crystals & a clear oil plus H20 condensation on top..the mixture warmed to room temperature turned back into a homogenous clear liquid..left to stand it crystalized as circular white dmt crystals with yellow cemicircular nmt crystals interlinked on top..

..update..the 'crystalized' material, upon being scraped from the dish became a
yellow>orange soft 'putty'..that's the nmt refusing to stay solid..however i suspect that the nmt as an oil is actually 95-98%nmt+something else (maybe betacarboline or 5meo-nmt or a plant oil)..re-purification of this putty/wax should result in a solid re-x of nmt/dmt, but may take away some of the extra 'character'..the crystalized nmt in the 2001 experiment went through two stages of purification/re-x, resulting in white 'swirly circular' needles that turned yellow upon standing..

..they are from another run on the same plant material around a year ago..the photo quality is not great, but it's something at least..
the friend estimates from simple chromatography that it is approximately 2/3 DMT: 1/3 NMT..

image shows the NP solevnt (dcm) after being left to sit after a small amount of H20 mist added and swirled..
due to NMT being more polar, a kind of very crude separation is seen between it (yellow) and DMT (white) ..
nen888 attached the following image(s):
pic#62.png (81kb) downloaded 1,405 time(s).
 
acacian
#46 Posted : 12/9/2012 7:31:47 AM

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ok so you remember that full spectrum extract i attempted a while back with the metho soak and then the presumed failed dry tek afterwards where i only got about 300mg of a sticky toffee? yesterday i noticed the bowl of sodium carb/dmt which i'd left sitting around still smelt unusually like dmt, so I added some isopropyl rather than acetone and did 1 pull and evapped.. ended up with some nice crystals. isopropyl seems far better for crystalisation than acetone which only produces a goo for me
 
thick-light
#47 Posted : 12/9/2012 4:49:59 PM

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So IPA pulls are resulting in better nmt crystalization? I have to try this on my reamining paste that is white but turns beige/peach upon a thorough drying, but still waxy and moldable. When smoked it melts like hash and kind of boils the dmt coated in nmt paste and results in a very potent experience. I think the nmt is encasing the dmt and allowing it to kind of simmer in the waxieness of the alledged nmt. The experience from smoking a nice ball of wax with dmt cryatals produced resulults that lasted 45-1:30 minute experiences that has drifting breakthroughs and an unbelievable tale that reminded me of psylocybin with a kick to it. After reading this thread I can't help but wonder if there are beta carbolines in the mix. I ended up adding 100 mgrams of sea salt to my acacia soup after an unbelievable amount of needle like dmt crystaals fell out of maybe 1/8 of inch of undecantd solvent. I heated the whole vessel with a space heater melting the dropped crystals back into the mix warm naptha was added along with 10 grams of Naoh and was then pulled while clear and hot. within 20 minutes the solvent was milky and more crystaline trees grew over a 6 hour period, once foze then scraoped produced a gooey needle straden goo that upon drying for a few days retained dmt crystal trees prouting out of peach/beige goo and when smoked were very tatsty. I really think I either have root bark that has a low nmt content, stem bark that has more dmt than nmt or that the naptha is being selective and sucking up the dmt first. Climate yearly conditions etc... could explain the nmt/dmt content if it is rb.I know you acacians nen, acacian etc... have been kind and caring in your reseacrh into these priceless trees, I would like to follow suit... Can you more experienced acacia extractors suggest any good books that might help me understand the array of alks that fill these trees and what climate produces low nmt in rb etc...

The 500 grams of ACRB????? is still yieldeding great results and I will defintely put it up on the wiki when I get the chance. Thanks in adavance for any insight you can offer Thanks...

I also wanted to note that the needle like crystals are almost like cotton in consistency and has this stringy quality to it, it is also decieving to the eye and seems like there's a lot more than there actually is.

I've been tryign To isolate nmt but was only able to do attain 3/4 of a gram to play with. This turned out to be very interesting and revealed a very different side to this tree that is mild with a mushy kick that is great
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acacian
#48 Posted : 12/9/2012 10:31:42 PM

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that was with a mainly dmt extract.. not sure what else could be in there
 
nen888
#49 Posted : 12/16/2012 12:16:39 AM
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..provided by above mentioned friend..photo of the NMT part of the above experiment, crystalised (after several days)
..is probably about 80-90% nmt..
nen888 attached the following image(s):
pic#71.png (196kb) downloaded 1,342 time(s).
 
Vodsel
#50 Posted : 1/16/2013 11:47:09 PM

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I'm leaving a little extraction report here since I don't think it deserves a thread of its own. Assays were basically negative, no further analysis conducted atm.

Species used: European A. saligna and A. retinodes, IDs obtained from the botanical information of the park where the material was harvested past december, in tentative small amounts. Pictures taken agree with the IDs.

#1 - A. saligna

100 g of dry phyllodes were crushed and soaked with ethanol/vinegar/water for a few hours.
The mix was brewed and 3 x acidic extracts were collected and reduced.
The rather thick acidic reduction was defatted with hexane.
Defatted mix was basified with lye water to pH 13+
First pull with hexane yielded after evaporation around 40mg of yellow resin not particularly promising.
Resin was allowed to dry completely, then infused into smoking herb.
Two consecutive assays with the equivalent of 10mg and 20mg were made, with no noticeable effects.

I still have around 50 g of twigs but the results with phyllodes are not encouraging, so I doubt it might be worth a shot. Also, I could do a second pull with DCM in the phyllodes extraction, but since hexane should work fine I do not see the point. Anyone thinks it's worth trying?

#2 - A. retinodes

50 g of dry phyllodes and small twigs were crushed and soaked with ethanol/vinegar/water for a day.
Mix was brewed 3x, acidic extracts were gathered and reduced.
Basification with lye water to pH 13+
One pull was done with DCM in a sep funnel.
Evaporation yielded some 80 mg of yellow/orange oils.
Oils were infused into smoking herb, which was assayed twice with 15 and 35 mg amounts. First was negative. Second had something to it, a mild buzz, but I'm very tempted to call it placebo.

In this case, I think collecting another small batch of retinodes leaves (maybe in late summer) and doing proper analysis might be worth it, considering there's at least one positive report of A. retinodes in Europe.
 
null24
#51 Posted : 1/31/2013 9:24:49 PM

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I plan on following the advice of Thicklight in your "having problems"thread. So far, there has been a little differntiation from yours though, due to newbiness. I did some really bad math and ended up soaking ACRB in a vinegar/water solution that was probably around 30% vinegar. This soak lasted for 3 days, then was decanted and more solution, at 10% vinegar was added to the bark.
Ok, SOOO, did the overacidification cause any problems I should be aware of? I did not rinse the bark or anything after decanting soak #1, and adding more. OK?
BTW, used a 1/4 lb of ACRB.
Next step in this experiment, plan on doing acid cooks at 1.5- 3 hours each, prol. 5 or so.
Sine experientia nihil sufficienter sciri potest -Roger Bacon
*γνῶθι σεαυτόν*
decrimART
 
nen888
#52 Posted : 2/1/2013 1:41:52 AM
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^..there should be no problem with that amount of vinegar..it is not a very strong acid in this form..
don't use math, use intuition..Smile

Vosdel wrote:
Quote:
In this case, I think collecting another small batch of retinodes leaves (maybe in late summer) and doing proper analysis might be worth it, considering there's at least one positive report of A. retinodes in Europe.
..thanks for your reports, which i only just noticed Vosdel..much needed research!
i recommend when first testing an acacia to test the small twigs, as well as phyllodes..that way, if there are alkaloids in bark more than phyllodes you will know (the small twig being usually the same content as main trunk bark, which of course is quite taxing to the tree to remove)
 
nen888
#53 Posted : 2/19/2013 3:59:34 AM
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mrfi wrote (in the info thread):
Quote:
1. Its stated a 70/30 methanol/water with a dash of vinegar is used to pull goods from material. Is the vinegar to make this solution acidic and if so to what pH level? Also can HCL be used instead of the vinegar to reach this pH level?

I think my confusion here lies with the fact that the tek states somewhere that the meoh/h2o + vin is better than just acidified water/heat for yield.

2. I have access to a reflux condenser/flask setup. Do i as opposed to boiling in pot, reflux the material for 30 mins or so then filter of soup, add new solution and repeat 2 more times then combine soup?

3. Most of the a/b teks ive read at this point say to reduce solution at this point, is this required with this method?

Also if i was to defat is that before or after reduction?

4. Would i then (reduced or not) basify to between 11 and 12.5 for final pulls?

5. Will shellite work for the defat and final pulls.?

6.Will toluene work for the defat and final pulls?


1. as stated earlier in this thread HCL is NOT good for acacia (reacts with other compounds) ..white vinegar, sulphuric or citric acids are fine..
2. refluxing is great/fine
3. reducing as much as possible means less NP solvent needed..more efficient, less wasteful..this is why defatting after reduction is better
4. 11-12.5 is optimal..up to 13 is fine..
5. shellite will work but is much less efficient than other solvents (i.e.) needs several washes/'pulls' to get all alks out at last stage
6 tolulene is, from what i know, a more efficient solvent to work with, but haven't personally used it..

best of luck with experiment..!
.
 
nen888
#54 Posted : 3/6/2013 3:29:17 AM
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..for acacias, reports indicate that the addition of table salt (as recommended by cyb in Cyb's Hybrid ATB 'Salt' Tek) to the basic solution prior to non-polar solvent extraction will help increase yields..use non-iodised table salt (finely ground)..

those using Acacia confusa..i would recommend the thick-light method described earlier this page..[#42]
numerous nexus reports have shown it to give good results..
.
 
Seldom
#55 Posted : 3/8/2013 12:29:29 AM

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pirateb0b i think one issue with FASA and acacias is that this method works best with smaller amounts of high yielding material. for 500g of phyllodes you would need quite a bit of acetone.

interestingly your own body produces acetone through decarboxylation of acetoacetate, and has been blamed for generating the fruity smell which poor people emit due to bad diets. Fumeric acid is produced naturally upon contact of the skin with sunlight. Citric acid is the only element of the equation which isn't endogenously produced!



limitless magnificence
 
acacian
#56 Posted : 5/10/2013 9:32:47 AM

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Mystery Acacia Extraction

-phyllodes were oven dried at roughly 100-110 degrees celsius for an hour and a half. the weight came out at 132g. the phyllodes were then ground to a very fine consistency.. not quite a powder

- the ground phyllodes were mixed with a generous amount (maybe 800ml) of cold water with a few squirts of lemon juice. final ph 4.

- the phyllodes were then boiled for a half hr. The liquid was poured off and decanted in the freezer for 15 minutes and then the fridge for 25mins. The liquid was then poured off and put in a separate pot to be reduced. another lot of water and lemon juice was added to the phyllodes and boiled for another half hr.. this was then decanted again and added to the previous boil to be reduced further. Filtering with cotton buds was performed at different intervals during the boiling process. this process was repeated 4 times

- the 4 combined boils were reduced finally to 300ml and filtered one last time with the cotton bud pressed firmly. the solution was left to cool down in the fridge for half an hour

- 100ml xylene was added to the solution and mixed thoroughly in a swirling motion for about 10 minutes. It was then allowed to sit until the layers had separated completely. the xylene was then pulled from the solution and discarded. it was a yellowy colour

- 6g NaOH was then stirred into to 100ml warm water and left to sit until the solution was clear (I wait for it to become clear so that I can spot signs of precipitation more accurately).it was then added slowly to the acacia solution. precipitates could be seen within a few seconds and the solution continued to cloud up as it was mixed. it then went a dark brown colour. the solution was left to sit for a half hr. the ph ended up at 12.25

- 100ml xylene was then added to the solution and then mixed in a strong swirling fashion constantly over the following 10 minutes. the solution was then left to stand and separate. the xylene was then pulled and kept aside in a flask

- 10g of NaOH was added to the acacia solution, this time without being dissolved in water first. It was stirred in until dissolved and left to sit for 10 minutes. another 100ml xylene was added. solution was mixed well for another 5-10 minutes and allowed to separate overnight. xylene was removed and combined with the first pull (all the pulls remained the same yellowy colour :/ .. much the same as with the last floribunda extraction

-xylene evaporated with hairdryer leaving an unpleasant smelling yellow film.. will bioassay tonight

photos of the acacia

notes: next time I will need to add less of the NaOH solution so that I can achieve a lower ph. I wasn't expecting the ph go to 12. my desired ph was 9. this also would have had to do with the small volume of solution. i had 300ml of acacia solution after reducing.. my initial intention was to do xylene pulls at ph9, 11, and 12.5
 
chocobeastie
#57 Posted : 5/13/2013 9:24:48 AM

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Nen,

I've never found any form of alcohol to be necessary for extracting from Acacias.

Normally, I use tartaric acid, as it is so efficient, and not very much is required.

Interesting to hear what you say about heat and acidity Nen, I always keep acidity quite low and minimise heating, only normally going to a light bubble (if that, especially when simmering down)

I find the first simmer will get 70-80% + of the alkaloids, and the 2nd may not even be necessary or worthwhile at times! (if you are dealing with a low yielding species)

Normally, the brew should be simmered down to a third of its original liquid volume. When you simmer it down too much, something seems to destroy the DMT, the heat or some sort of chemical reaction? I don't know, but avoid too much heat! and acid!

Then Sodium Hydroxide added slowly as the granules, stirring, watching the colour change go white (the longer it stays white the higher the yield it seems), then dark, then black. When it goes black, add a third as much Lye again, that will normally bring it up to around 12.5, which I have found optimal (back when I had a crazy precise PH meter ;-)

So then if I had a 1 litre-1.5 litre of liquid in a jar, simmered down from say half a kilo of phyllodes, then I would add 100-150mls of Toluene, stir for a few minutes briskly and repeat this step two more times. I used to shake, but quick stirring really does the job!

Then if the solvent is really yellow and needs cleaning, I will do a water wash with a few sprinkles of lye, another wash with a tiny pinch of Bicarb and another wash with just water.

If it looks really clean, I'll just do 2-3 water washes, and then let it settle for up to an hour.

I recently tried using Xylene and didn't like it, too toxic!

With Toluence, the alkaloids will dry as an oil and then normally dry into an opaque crystal. You NEED to use a fan to dry it, it only normally takes overnight with a fan.

I find toluene works very well, but of course d-limonene pulls major full spectrum alkaloid goodness! ;-)

Also, Shellite is only really useful for extracting out pure DMT crystals or for recrystallisation and I reckon Shellite sold these days in Australia is basically almost useless for extractions. I swear it used to work! ;-)

Also, Nen, I would be interested in seeing photos of those Maidenii's, and what time of year was this? It would be good to get more information about what time of year and what strains are active in what places and how to find them.
 
nen888
#58 Posted : 5/13/2013 9:42:08 AM
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..first up acacian..i think your mystery acacia may be Longifolia..
any pods yet?

hey there chocobeastie..thanks for your comments and info..
you're right alcohol is not essential, however i suspect it can increase yields (being a very efficient solvent for tryptamines in general) .. but not essential, yes..

i'll see about getting some photos of the active Maidenii's..general area is s.e.qld..time of year when drier..
the ones i know look a lot like the narrower phyllode melanoxylons in the area, though Spice Sailor posted pics ages ago in the info thread of an active broader leaf type in the same area..though i wonder sometimes to what extent it is individual trees rather than many with some of these species..


 
jamie
#59 Posted : 5/13/2013 4:56:56 PM

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I extracted some phlebophylla phyllodes some awesome wizard sent to me recently, from dead phyllodes off the ground..

I just sort of made up my own tek as I went.

I brewed the phyllodes in vinegar water 3 times, and then reduced it and evaporated it down to the point where it was almost dry in my dehydrator..then based it with calcium hydroxide and then fully dehydrated it after mixing it around and leaving it to base for a bit.

Then I crushed up the based powder and pulled 6 times with sunflower oil..3 of those pulls were hot sunflower oil..

then I collected all the pulls together and salted them 3x with vinegar and water..evaporated the DMT saturated vinegar water down to a goo, and then based the goo with sodium carb and water and repulled it when dry with 99% iso..and evaporated.

Worked for me anyway..stuff feels practically identical to mimosa spice for me and is very clear and crystaline and deeply euphoric..very much unlike other non mimosa sources like chaliponga and wild grass.
 
acacian
#60 Posted : 5/13/2013 11:55:28 PM

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..sure sounds like a friendly wizard to me Jamie. Smile I wonder however, whether the smaller yield could possibly be attribute to the large amount of acid used? You only used vinegar right? people have mixed results with acacia when using too much acid and sometimes find reduced yields.. I am not exactly sure why this is, though I am sure nen or choco could elaborate? below an extraction of my own.. next will be mucronata. I'm just trying to figure out whether to gather the phyllodes today or after a longer period of no rain..

Acacia Floribunda extraction

Phyllode length = 12.5-15cm
Phyllode width = 0.5-1cm (phyllodes were larger the further down the stem)
Flower rods = 4.5cm .. very abundant
No basal gland
small white hairs present on phyllodes and stems
Rough trunk bark (observed often in the commercial varieties of floribunda grown in urban environments)

-Phyllodes and developing flower rods(not yet in bloom) were oven dried at 120 degrees celsius for an hour. the weight came out at 171.75. the phyllodes were then ground to a near powder. meanwhile as the phyllodes were drying, the twigs and stems were boiled whole for 2 hrs in water with a squirt of lemon juice

-A generous amount of water and a squirt of lemon juice was added to the ground phyllodes in a saucepan and boiled twice for an hr each. each boil was decanted. the first two boils were combined and filtered through cotton buds. the 3rd was brought to the boil and left to sit for 24 hrs before being poured off filtered and added to the previous two. the water from the twig boil was combined with the three boils at the end and reduced down to 400ml.

- 100ml xylene was added and mixed well in a swirling motion.. it was given a heat bath to speed the process as it was not separating well. the layers separated after 10 minutes in the heat bath. the xylene was then pulled from the solution

- 25g caustic soda was dissolved in 150ml warm water and left to sit until the solution was clear. the solution was then added to the acacia soup. precipitation was noticed as it was added and continued to do so while it was stirred for about 10 seconds before disappearing. however, the solution stayed a very light brown colour even after ph 12.5 had been reached. the solution was left to sit for 20 minutes

- 100ml xylene was added to the solution and mixed thoroughly in a swirling fashion, allowed to stand and separate and then pulled from the solution. It was a murky yellow colour. the xylene was left overnight and evapped today.. not looking like there's anything of interest.. a very slight yellow film again which I'll bioassay. it could be the weather in the melbourne, but I really don't think floribunda is a particularly reliable source for dmt at all. i think it must be a certain strain of it that is active.. i have done well over 20 floribunda extractions down here at differen't times of year and never gotten dmt. the yellow film smells similar to the stuff from the last extraction.. i wonder if this is a common chemical that occurs within species in certain environments or weather patterns

Notes:
-before the xylene was added, the basified solution was still quite light in colour - as it was tipped from side to side precipitates were observed and it was assumed that they were making the solution lighter in colour. After adding the xylene and mixing/separating, the solution turned to a very dark colour
-upon closer inspection tiny cream coloured particles could be seen floating in the xylene which was quite cloudy. could this perhaps be an alkaloid becoming insoluble as the xylene cools down in the cold atmosphere?
 
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