Acacia Simplex - STB Extraction and Experiments

[pastanostra]

Hi Nexians, wish you a nice start in this year with beautifull things. Our start gived us some way, in life, health and a direction for the future.

We started our first extraction using a very very lazy way, the tek was inspired from the lazyman tek and advice of Godsmacker.


The Simplex is gived for 3,6% of Alkaloids in bark, the old study report in trunk bark ~40% of NMT, ~20% of DMT & ~12% of beta carbolines.
Actually we have no way to analyze this content, our only way to analysis will be eye observation, and a scale (normally mg scal but it actually come from china at low cost )

Cooking


We started mesuring out 51g of Simplex Bark

We mesured 60g of Lye and carefully added it to 500mL of distilled water, then added to the bottle with the bark, let's say at D0 8:00PM the basic soup is done. So the process really start.

The soup began purple / dark in few minutes, the soup was gently stirred during above 20/30minutes. The soup sitted overnight in a dark place.


The next day à 1:00PM we've done a heat bath with stiring.
We can notice during heating that the color of the soup turn to dark / purple to orange

The next day at 10:00AM we've done a heat bath with stiring. At this stage, we added 50/70mL of clean Petroleum Ether. Stirred nicely, for the naphta can get down to the basic soup and can ascend the soup gently. We repeated this process 4 times.


The next day at 12:00AM we poured out above 30/50mL of naphta an putted in the freezer overnight.
This pull has no pics but ended with 400mg of white powder. The naphta was recycled andslightly yellow


After the 1st pull, the soup was heated, recybled naphta was heated at the same time and putted together in bottle. We stirred during one hour at heated bath temp (~50-70°). The soup sitted overnight, while sometimes stirring during 20/30minutes.

At D+3 5:30PM the second pull was pourred out and mesured above 100mL. A bit of wind clouded the naphta.
After freeze precipitation, we ended with nice white xtalz et yellow goo/powder

During the drying process of this pull, the yellow part of this extract, melted at room temp, but while scrapping it become solid. I believe it's the oily film that trapped some solvent & water (there is above 80/90% of humidity in the air at home). The pull finally stated in a pretty yellow powder that smell dmt and some tanins of forest

In the picture below you can see the difference between pull N° 1 pull N°2, the 1st pull hasn't been heated at all (room temp ~28°)

We ended with above 900mg of yellow spice

For the 3rd pull, we recovered used naptha (160mL) and added to the soup. Heated it for 2 hours, stirred & let it cooled at room temp. This has been done 2 times in ~24h.

At D+4 5:30PM, after the last heat bath / stiring combo cooled, we poured out the naptha (~130mL) in a dish, evaped above 20mL before the solution become cloudy. Let it sitted in freeze for 26h.

At D+5 7:30PM we poured out the solvent from the dish, and let it dry.


We can see nice xtal formation, as the freezer was less been used during this time unlike the other pulls. It increase significantly the beauty of xtalz formation
We can notice too, the gooeyish film at the bottom of the dish, i believe it this one who melt the xtalz because it trapp solvent.

We weighted above 500mg of nice yellow powder that smells like the pull n°2

At D+15 we've done 3 heat bath, the naptha was so fatty that it had some hard time to get up the bottle. This has been freeze precip. in 24h and dried on a goo state. During scrapped this goo dried ina yellow powder, like the pull before (2 & 3).
Ended with 500mg.

Some infos

At this point, we're above 2,3g of 4 pulls, with 51g of powdered bark. This represent a yield more than 3,6%.
We considered have used used naptha that can contain a bit % of goods. It's the most inacurate element in the whole process. The scale is a bit inacurate too let's say 0,015g.

For sure heat during pull help to get more goods, there were no salt added, i believe the salt help speeding the process.
Our precedent extraction was The Cyb's hybrid AB tek. The "crude extracted spice" was less yellow (comparing the 4th to 6th pull with used solvents).

An interesting point, the finals combined extracts don't melt at room temperature. Can you consider there are not a lot of NMT in ?



Cheers all.

 

[Godsmacker]

First of all, THANK YOU FOR TAKING THE TIME TO SHARE YOUR RESULTS WITH US!

I am glad to see that my advice has been of use in your investigation! I oftentimes find that a long, protracted STB with six to seven pulls collected over a week or two tends to get larger yields than normal. This may be because more actives leach out into solution the longer the bark has been sitting in a concentrated/caustic NaOH solution for. I commend you for your patience, and am surprised that your unrefined extracts (post freeze precipitation) were solid, whereas my only past (and failed) simplex bark trunk bark extraction, alongside every A. Confusa root bark has yielded a sticky waxy viscous 'goop' after freeze-precipitating. I think this may be because I live in an extremely humid area, and thus freebase tryptamine crystals tend to turn into goo after sitting at room temperature for a few minutes. I am astonished to see that you were able to get an extract of yellow spice which remained solid after freeze-precipitation, and commend you for that.

I would suggest using heptane/hexane (or fresh naphtha) to recrystallize the contents of each pull you noted; I would like to see how recrystallizing/purifying may change your yields and product.

With respect to your used naphtha, I would suggest salting out any spice left behind via slowly adding FASA (Fumaric Acid Saturated Acetone) to the pooled pulls at a rate of ~1 to 5 ml per minute, gently stirring the solution with a glass rod as it is slowly added (ALWAYS USE GLASS VESSELS WHEN HANDLING ACETONE AND/OR PETROCHEMICALS). It should be highly noted that ONLY anhydrous acetone will work for this technique, as
the water present in non-anhydrous acetone would make the fumarate salts soluble in FASA. To combat this, I always add a generous sum of ~30 to 50 grams of freshly-baked MgSO4 to 1 L of ACS/USP-grade acetone to keep it anhydrous, shake it up for a few minutes, then add enough fumaric acid to get a 5 to 10 mg/ml solution of FASA' allow a day or two with occasional shaking to fully dissolve fumaric acid.

If the naphtha solution doesn't get cloudy (or any precipitate observed) within a minute or two after/during addingincrements of FASA, nearly all product has been salted out of solution. Carefully decant (or evaporate) the acetoneetrochemical solution, let extract dry and weigh. After this, I would suggest purifying the crude fumarate precipitate according to this thread, recording dry mass and other characteristics of product as it is purified, making special note of final mass.

I would like to see how such purifications/re-crystallizations of the freeze-precipitate and salted-out fumarates would impact quantity/potency and looks of product. I wish you well in your investigations.

 

[pastanostra]

Hey,

Thank you for your message.
I gonna see to check pricing of theses chemical to try it definitely

At home, during these extraction, T° was above 28°C and 85%+ humidity.
I believe the trees give differently between seasons / age / environmment. In a further harvest, maybe trying phyllodes on this tree, bark on another tree location, trying same season will report to nearly one year, but trying to get same conditions (uppign moon, no rain during many month, heat ..) to compare what product we can obtain...

Please find below 2 photos of the pull N°4 :

the goo who became solid during scraping

the solidified goo to powder

So actually combined extract weight for ~2,3g.
I wish planning to re-x with naptha. Do you think it's better o do a "general" re-x or multiple re-x (understanding all combiened extract in one re-x step) than multiple small re-x (500mg per 500mg) ?.

Cheers all

 

[pastanostra]

Hey There, a small update :

At D+21, after 3 heat bath and stiring, let it cooled, pulled 50mL of naptha.
After 36h freeze precipit, end with 180mg of brown extract.

First picture, with 3 type of extract, from the left to right : pull 01 - pull 2, 3, 4 - pull 5.

Second picture, you can notice a layer of sorts of fat (above 1cm). The more we stir, the the more it's harder for the naptha to come up (this one crashed of the soup during the freeze precip.). This layer is naptha soluble, at room temp and heat. The last pull (N°5) maybe have trapped this fat and this is why it's brown (cause no decant was done, maybe ...).

For the last pull i'll don't take this fat (let it decant during some days then pour the naptha out)

 

[○]

Awesome job pasta! Beautiful

Now a vape report is needed. :grin:8)

Cheers

 

[Nereus]

With respect to your used naphtha, I would suggest salting out any spice left behind via slowly adding FASA (Fumaric Acid Saturated Acetone)

I can hardly believe that using any kind of FASA/I to salt alkaloids out of naphtha would work. In my experience, fumaric acid dissociates from the medium it's saturated in after adding it to pet. ether, making it crash out of solution. Correct me if i'm wrong, but my experiments showed that FASA/I in naphtha does not work.

 

[Godsmacker]

With respect to your used naphtha, I would suggest salting out any spice left behind via slowly adding FASA (Fumaric Acid Saturated Acetone)

I can hardly believe that using any kind of FASA/I to salt alkaloids out of naphtha would work. In my experience, fumaric acid dissociates from the medium it's saturated in after adding it to pet. ether, making it crash out of solution. Correct me if i'm wrong, but my experiments showed that FASA/I in naphtha does not work.

Have you tried evaporating nps post freeze=pprecipitation in a cylindrical glass container until >10 to 20 ml of fluid are left, then apply FASA? I have never tried this, but it would be cool to see what happens if you use FASA on a very small volume (10 to 30ml) of naphtha post freeze-prcip.

It's worth a shot

 

[Godsmacker]

For the purpose of keeping records, I would highly recommend you maintain lab notebooks pertaining to your progress. I have attached one (or two) guidelines for maintaining a lab notebook below

http://www.training.nih.gov/assets/Lab_Notebook_508_(new).pdf

http://web.mit.edu/me-ugoffice/communication/labnotebooks.pdf

Experimental biosciences laboratory resources <---- this is one of the better guides on keeping a notebook


Please keep quality physical lab notebooks (& Scanned copies of pages if you'd like to make .pdf copies to share ), copies of everything and all data, too. One can avoid a lot of legal bullshit if they can produce evidence of the conducting of a professional scientific investigation.

I am very proud of the time and effort you and your colleagues are putting into this project, and I am ecstatic to see where this will lead!

Godspeed,
-Godsmacker

 

[Godsmacker]

As an aside, is it the dry season in New Caledonia? I would appreciate it if you may be able to harvest some fresh & dead bark/branches/seed-pods/phyllodes/etc. during the peak of the dry and wet seasons, in order to see if rainfall may influence alkaloid content, as it has been noted to with other plants.

 

[pastanostra]

Hey there, thank you for your messages.

So, what i suspected was really, the 5th pull was basic soup contaminated.
The fault was at the new turkey baster received, too much pressure ...

I had a little bit fresh naptha, just the necessary to do a mini a/b.

As the five combined extract was contamined i started to do a re-x and to a 6th pull. As it's rainy, the week end is chemistry.

We weighted our 2,5g combined extract et dissolved it in 300ml boiling naptha.

We can notice the waste at the middle of the jar. The color of naptha is pretty yellow, but cristalline

We separated the naptha and can noticetha was basic soup and some more fat (tried by contact, picture aren't awesome).

Then we putted the naptha in acidic solution (250mL water,20mL acetic glacial). Notice the color change and opacity of the naptha.

The solution was stirred and sitted during an hour, then the pahta pourred out in our recycling jar. We can notice that acidic solution is not translucent (tinted by a bit yellow)

At this point, we didn't know how aqueous phase can be saturated or if it's already saturated. We decided to add more acetic acid (+200mL water + 15mL acetic). The naptha was pulled in the acid jar, then stirred nicelly, then pourred out the naptha.
We can believe that all DMT is in the acidic solution.

This was followed by adding basic mix (250mL water, 45g lye) into the acidic solution.
At our surprise it was like the milky way, turned like milk (if there no dmt smell, we should believe that it's milk)

On this dmt milk, we've done 5 pull that ended the bottle nearly clear. (the small parts on the side of the jar are fat fragments of t he biggest mother fat in the middle).

The nearly water clear mix, sitted overnight.

During this time the 5 first pull were in the precipting dish, but this time let's try growing nice xtalz.
Note : Until the 5 pulls have been done, some crystal precipited at room temp without evap, theses are reflecting like precious stones. The naptha is a bit yellow.

The five pull sitted overnight at room temp, in the morning we decided to put a seed inside the dish and will see ..

The things you see a bit brown are the plate under the dish that got marks. We can see the "seed" up to the center of the dish.

This dish will sit 24h more here, then will be carreful put in the top level fridge, then going down everyday, the finish in the freezer for 2 days.

In the morning, we were surprised to see some precipitation in our basic mix . Check this cassoulet, you can see precipitats floatting in the aqueous mix, there are bit particle, and some very small. Notice on the second picture the nice 3 layer mix, naptha (yellow), fat (white), aqueous mix (translucent with precipitats).

We heated a bit the mix, all precipitats rounded inside the jar but didn't disapeared.

We decided to do a 6th pull to clean up this mix...

The aqueous mix seems to be cleaned by solvent, we can distinguish the fat layer and the solvent very yellow.

This 6th pull is in the freezer for freeze precip.

With 2,5g at start, we'll see how we get at the end of Mini AB.
With that, we can consider have epured and lost a bit of product, some fat and other waste are throwed. Can we consider other thing ?

On the main STB, we've done the 6th pull, taking care of basic mix. This pull has been put in a white ceramic dish, the pull turned nicely cloud (seen a mixed yellow of eggs).
Tomorow we'll see the results.

We've finish with this STB, the basic mix has been trowed as we have no more naptha. We're pretty sure that there were some bit more good inside.

Thank you Godmsacker for these helps, the lab notebook is done on this 1st experiment, but not rich as in the how to.

In our next extraction we'll carefully take care of it.

With these small experiment, i find naptha is a problem, cause it's expensive, and we use a lot of it, for nice results, clear naptha has to be used. We can use naptha that is used for pull, but it's evident the pull will get some of the fats or other compound in the extract.
Recycling it with a DIY alambic seems to bee dangerous as i don't know the reaction with copper .. Can't consider that.

FASx teks seems to be the way, but depend from chemicals too. Old culture use the nature for that. This tree is growing near the sea.
The sea is water + salt (+ living things inside), maybe it can be a starting point for sustainable process. I think i remember from school that salted water is good for electrolyze. Can a reaction with lectrolyze alterate bark or it's content ? Can it change structure of DMT ?

I heard a bit about silver colloidal. This principle seems to in distilled water (so witout ions), put by electrolyze to put inside the solution positive silver ions. This seems to put the in the water a certain potential in chemical activity to grab negative ions off things.

As there is a lot of knowledge inside dmt-nexu community, can somebody know if it can do something to bark ? or acidid solution ? or basic solution ?

Considering another, if we take bark, we put it in an alambic and distillate it, what can we obain ? I believe a bit of essential oil but what else ?

Thank you all for your readings and lightnings and I apologize for every mispelling, writing faults ...


Cheers all.

 

[Nereus]

I'm becoming very curious about your end result after all the processes involved, pasta. Thanks for taking the time to keep us updated!:thumb_up:

 

[Nereus]

With respect to your used naphtha, I would suggest salting out any spice left behind via slowly adding FASA (Fumaric Acid Saturated Acetone)

I can hardly believe that using any kind of FASA/I to salt alkaloids out of naphtha would work. In my experience, fumaric acid dissociates from the medium it's saturated in after adding it to pet. ether, making it crash out of solution. Correct me if i'm wrong, but my experiments showed that FASA/I in naphtha does not work.

Have you tried evaporating nps post freeze=pprecipitation in a cylindrical glass container until >10 to 20 ml of fluid are left, then apply FASA? I have never tried this, but it would be cool to see what happens if you use FASA on a very small volume (10 to 30ml) of naphtha post freeze-prcip.

It's worth a shot

Here is a thread discussing the above subject of adding FASA/FASI to dmt staurated naphtha.

Contrary to my findings, Nitegazers experiments seemed to have worked. Regarding this matter i've come to the conclusion that the potential success of this experiment could also rely on the actual hydrocarbon composition of the used naphtha. And i can only say that the brand i used to employ the FASI technique (equal parts pet.ether, pentane,heptane) made most of the fumaric acid crash out of the FASI shortly after the two mixed. I'm taking back the statements in my previous post.

Godsmackers point is quite interesting actually, in that any potential actives left in the nps could be pushed out using this method, being simple enough and accurate too. It's a good idea and, yeah, worth a shot. :thumb_up:

 

[Godsmacker]

PLEASE USE A GRADUATED GLASS PIPETTE. NOT A GLASS TURKEY BASTER :!: :!: :!: :!: :!: :!: :!: :surprised

Graduated Glass pipettes (10 ml) are xtremely cheap and are far more efficient at transferring liquids. Far Far Far less drips out each time you transfer liquids.

Maintaining a lab notebook is an art; one can only learn by doing.

 

[pastanostra]

For sure, I learned that

In waiting of the rest, we can see our 6th pull of the mini AB (150mg) :

Cheers

Note : just some xtals - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus

 

[pastanostra]

Hey There,

So a bit news of the washing-re-x.
We ended with 1700mg of yellow salt rocks. our freezer has been too much used during this time... So we have loss 800mg of unknown component.

Here you can see the 6th pull of the mini ab (rapid freeze precip) andthe 5th combined first pull of the mini ab (slow freeze precip).

And a texture comparison with our first experiment in mini ab.

We'll not go further in washing theses xtalz.

We actually tried a tek with vinegar / sodium carbonate / IPA or Ethanol.
This seem very very promising because the simplex seems to have many ressources in him.

Tis pic is a crude (so crude) extract with ethanol, this has not been filtered and was causing us some trome fo the next steps.

This endedwith a very crude black extract that smell so sweet, it smeel flower, forest, but everything is so sweet.
This extract has been burned tested and, smell so nice, and dmt in the background. The first smelling are flower and tree spirit.
At this point the exract is bit fucked because it has not been carefully filtered. it contains plants materials. We tried too clean a bit, butwe don't arrived cause of sodium carbonate that don't dry... (tried multple wash but always ended with sodium carbonate at the end).

We started an another extraction with this cool tek, and took care by fully decant / filter the pull. The IPA solution is very clean (translucent). Actually 2 new pulls are decanting / filtering. Will update with pics later.

Cheers all.