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I think I messed up my first FASA Options
 
AIRDOG
#1 Posted : 2/16/2015 4:56:06 PM
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Hi how are you my fellow nexians!!! i have learnt a lot over here so i want to give a big thank you to this awesome community of travelers...

In the past i have experimented with q21q21 dry tek and CYbs salt and max ion teks.... i have had some decent results but i thought i could have some yield loss because of using old oxidises bark...

So i set up to make a new extraction this time using q21q21 dry tek but using a broader spectrum NPS... TOLUENE so i can get the oxides out in order to do zinc redux but i think i messed up in the FASA step, i kinda have the idea of what could have been wrong but no sure...maybe you could give me a better clue of where i messed up and how can i solve it:

1. Used too much toluene or it was not saturated enough...
2. Acetone not dry (3.5 grams fumaric to 50 ml acetone) it did not dissolve much of the f.a. apparently
3.used to much fasa?


Materials:
100g MHRB
100g calcium hydroxide
100 ml water
200 ml toluene

My steps were:

1. 24 hrs 50/50 water/vinegar soak
2. Mixed the lime and let set 6 hrs
3. toluene pull 100 ml (it came out clear)
4. let sit overnight
5. Toluene pull 100 ml (came slightly yellowish but clear)
6. add pull 1 to pull 2
5. add FASA to toluene
7. since nothing seemed to precipitate I added more fasa and then shaked the bottle...
8. bottle turned cloudy and i put it to evaporate right now

i dont know if someone can give me some insight as to how to fix this???

My first guess is i will have to evap the FASA/toluene mix, add small portion clean toluene to dissolve leftovers, filter fumaric acid dust, add more fasa? repeat?

please can somebody helpful point me the right direction??

thank you so much!
 

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concombres
#2 Posted : 2/16/2015 5:20:28 PM

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Did you dry your acetone with magnesium sulphate?
 
AIRDOG
#3 Posted : 2/16/2015 5:22:33 PM
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no, i read in other post doing such is overkill
 
concombres
#4 Posted : 2/16/2015 5:46:46 PM

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AIRDOG wrote:
no, i read in other post doing such is overkill


Dry some acetone, evap your tolulene & scrape your full spectrum.

Once the acetone is dry dissolve your full spectrum in a small amount & use the rest to make fasa.
Drip it in slowly a few mls at a time, if no clouding occurs, come back here.

If clouding does happen, wait for it to dissipate & add a few more ml fasa, repeat.

Dont shake & dont rush. Adding it too quickly will get you goop.


 
AIRDOG
#5 Posted : 2/21/2015 2:08:23 AM
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thanks!! yo u have been most helpful!!! i have seen that the goo is starting to crystallize... i didnt know i had to wait so long...

after reading and studying many hours in the forums, i think im going to use DCM for making pulls from the paste as i have read that it effectively dissolves all alks in less pulls... steps would be like this

1. pull from lime paste with dcm
2. evap and scrape
3. dissolve crude in vinegar
4. reduce with zinc
4. base with lye
5. pull with toluene
6. fasa
7. wash with dry acetone
8. base with sodium carb
9. retrieve freebase dmt from the sodium bicarb paste with dry acetone or IPA
10. evap to leave a clean product maybe

I think i have it nailed... but does it sound right?? im about to do the dcm pulls so i still got time for some answers
the truth is im looking for high yield of white pure crystals...


 
concombres
#6 Posted : 2/21/2015 2:46:23 AM

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AIRDOG wrote:
thanks!! yo u have been most helpful!!! i have seen that the goo is starting to crystallize... i didnt know i had to wait so long...

after reading and studying many hours in the forums, i think im going to use DCM for making pulls from the paste as i have read that it effectively dissolves all alks in less pulls... steps would be like this

1. pull from lime paste with dcm
2. evap and scrape
3. dissolve crude in vinegar
4. reduce with zinc
4. base with lye
5. pull with toluene
6. fasa
7. wash with dry acetone
8. base with sodium carb
9. retrieve freebase dmt from the sodium bicarb paste with dry acetone or IPA
10. evap to leave a clean product maybe

I think i have it nailed... but does it sound right?? im about to do the dcm pulls so i still got time for some answers
the truth is im looking for high yield of white pure crystals...




I can't comment on using dcm as a solvent because i've never used it.
One thing i will say is i remember reading talk about dcm reacting with dmt to form a chlorinated dmt compound of some sort after sitting for so long so it may not be the best option.

I did yeild a goo with FASA not long ago & cleaned it up in a way very similar to the way you describe & it worked well.

If you'd like i'll link you to the thread. I made sure to document what i was doing as it happened to remember exactly where i was in the extraction & also to help anyone else who may run into the same problem & have trouble finding the info Big grin


 
AIRDOG
#7 Posted : 2/21/2015 3:41:48 AM
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concombres wrote:

I can't comment on using dcm as a solvent because i've never used it.
One thing i will say is i remember reading talk about dcm reacting with dmt to form a chlorinated dmt compound of some sort after sitting for so long so it may not be the best option.


I had read that today already, and i think endlessness had proved that to be wrong info, but regardless i do not intend to leave the dcm sitting there... im gonna evap it as soon as i make the pulls

concombres wrote:

If you'd like i'll link you to the thread. I made sure to document what i was doing as it happened to remember exactly where i was in the extraction & also to help anyone else who may run into the same problem & have trouble finding the info Big grin


thank you i would like the link if you please!
 
concombres
#8 Posted : 2/21/2015 3:50:32 AM

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AIRDOG wrote:
concombres wrote:

I can't comment on using dcm as a solvent because i've never used it.
One thing i will say is i remember reading talk about dcm reacting with dmt to form a chlorinated dmt compound of some sort after sitting for so long so it may not be the best option.


I had read that today already, and i think endlessness had proved that to be wrong info, but regardless i do not intend to leave the dcm sitting there... im gonna evap it as soon as i make the pulls

concombres wrote:

If you'd like i'll link you to the thread. I made sure to document what i was doing as it happened to remember exactly where i was in the extraction & also to help anyone else who may run into the same problem & have trouble finding the info Big grin


thank you i would like the link if you please!


the dcm should work fine then Smile
You seem to have done your research very well.

cleaning FASA

If you run into any further trouble keep posting here & i'll do as much as i can to help you get nice clean spice Thumbs up
 
AIRDOG
#9 Posted : 2/21/2015 5:06:10 AM
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well i just made the DCM pulls....

Used 400 ml for each pull on 500 g MHRB

i was able to recover 400 ml from both pulls so half of the solvent was "lost" but its almost already done evapping with my big fan...

I can already see some spice stalagmites forming!!! so awesome

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AIRDOG
#10 Posted : 2/21/2015 1:17:18 PM
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today i woke up to see with dismay that all the crystals that were forming are gone... and there seems to be some liquid like water on the evap dish... I dont know what it is...

does DCM seem to have a lot of water content??' the shit did not evaporate overnight.... but it no longer stinks like dcm....

im just gonna wait for it to completely evap to see if those cristals come back or i will only get goo....

that is really getting to me.... how come xtals just dissapeared??
 
concombres
#11 Posted : 2/21/2015 8:06:13 PM

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AIRDOG wrote:
today i woke up to see with dismay that all the crystals that were forming are gone... and there seems to be some liquid like water on the evap dish... I dont know what it is...

does DCM seem to have a lot of water content??' the shit did not evaporate overnight.... but it no longer stinks like dcm....

im just gonna wait for it to completely evap to see if those cristals come back or i will only get goo....

that is really getting to me.... how come xtals just dissapeared??


Solvent could have picked up water from the basic phase.
Could also be liquidy from other alkaloids & oils/fats. It will crystallize once it's pure enough.
The reason dcm works so well is that it is a less selective solvent & dissolves alot more than just dmt & it does it extremely well (meaning not just dmt but also fats oils, etc. are extremely soluble in dcm, the exact reason freeze precip wont work with it.)

Just let it finish up drying & proceed, your on the right track Smile
 
AIRDOG
#12 Posted : 2/23/2015 3:57:13 PM
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Okay so I ended up with some soft amber oil... which i dissolved in vinegar and did reduction on.... later i filtered it and added lye water so the vinegar turned milky and some fatty tissue precipitated which I believe is a saponification reaction...

now my question is if I should decant this fatty stuff before pulling with dry toluene...
 
concombres
#13 Posted : 2/23/2015 8:41:58 PM

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AIRDOG wrote:
Okay so I ended up with some soft amber oil... which i dissolved in vinegar and did reduction on.... later i filtered it and added lye water so the vinegar turned milky and some fatty tissue precipitated which I believe is a saponification reaction...

now my question is if I should decant this fatty stuff before pulling with dry toluene...


Try to get the fatty layer out & save it. You may be able to recover dmt from it later.
Proceed with a few tolulene pulls on the clean liquid & salt out with fasa Smile
 
AIRDOG
#14 Posted : 2/26/2015 3:51:21 PM
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well hi!!! i did a trial salting with small amount of solvent, and i was very happy with the results... altough i think i messed up and added too much fasa once because of my sloppy hand with the baster... (need to get a dropper)

As i saw this result i proceded with remaining tol very carefully and the results are much better... I dont know how to thank you for all your help conconbres!!!

im truly amazed by the result... now i only need to wash... ill post more pics when its done

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concombres
#15 Posted : 2/26/2015 8:23:01 PM

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AIRDOG wrote:
well hi!!! i did a trial salting with small amount of solvent, and i was very happy with the results... altough i think i messed up and added too much fasa once because of my sloppy hand with the baster... (need to get a dropper)

As i saw this result i proceded with remaining tol very carefully and the results are much better... I dont know how to thank you for all your help conconbres!!!

im truly amazed by the result... now i only need to wash... ill post more pics when its done



I use a teaspoon to drip the fasa in in small increments. Much less leakage than a baster. Thumbs up

Looking forward to seeing your results Smile





 
AIRDOG
#16 Posted : 3/7/2015 4:16:37 AM
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Well i made 2 pulls.... and these are the fumarates....

the second picture is a precipitate that formed in the dry acetone I used to wash the fumarates...

is it DMT???
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DSC08010.JPG (1,703kb) downloaded 68 time(s).
 
concombres
#17 Posted : 3/7/2015 7:45:15 AM

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That should br your dmt fumarate Big grin
You wash with dry acetone because the dmt fumarate is not soluble but the excess fumaric acid is.

Are you looking to store it, use it orally, or smoke?

If you want to smoke it just mix with sodium carbonate in a 1:1 ratio, add water dropwise until it's a paste & let it dry, then wash 3x with cold water. Precipitates will be dmt.

You can further clean it by re-basing as mentioned above, washing with water, re-FASA, wash with dry acetone 3x, then re-basify for smokable product or leave as fumarate for oral use.

 
AIRDOG
#18 Posted : 3/7/2015 2:34:04 PM
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im gonna keep half of it or a little more of it in its salt form for long term storage, the other part im gonna use it for rocket launching to hyperspace (I hope)

I already added sodium carb saturated water dropwise to some fumarates i dissolved in little warm water.... it clouded heavily, and i placed it in the fridge... i can already see some yellowish rocks forming...

I know the first picture are fumarates... the sketchy product is in second picture the one that has 1 bottle by itself?

look the rhomboid crystals?? those precipitated out of acetone that i used to wash the products of the petri and the bottle in the first picture... not sure if those are dmt fumarate too or fumaric acid crystals...

 
concombres
#19 Posted : 3/7/2015 3:20:17 PM

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AIRDOG wrote:
im gonna keep half of it or a little more of it in its salt form for long term storage, the other part im gonna use it for rocket launching to hyperspace (I hope)

I already added sodium carb saturated water dropwise to some fumarates i dissolved in little warm water.... it clouded heavily, and i placed it in the fridge... i can already see some yellowish rocks forming...

I know the first picture are fumarates... the sketchy product is in second picture the one that has 1 bottle by itself?

look the rhomboid crystals?? those precipitated out of acetone that i used to wash the products of the petri and the bottle in the first picture... not sure if those are dmt fumarate too or fumaric acid crystals...



When you wash with acetone you want to rinse your product in it, filter, & keep the solids. That is the dmt fumarate.

The sketchy stuff you can run through a few more dry acetone washes & if it doesn't dissolve completely with 3 washes it's dmt fumarate.

It may be fine dmt particles that crystallized over time & fell out of solution.

 
AIRDOG
#20 Posted : 3/13/2015 1:49:22 AM
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Hi!!! im sorry i neglected the extraction and thus this post... this is what i got... i have some more saturated solvent im gonna fasa later... and some fumarates

I converted my first fumarate pull to free using saturated carbonate water added dropwise in fumarates dissolved in water....

somehow im not sure if all of it is dmt... i think i have also sodium carb xtals because of the color differences in xtals in there and also got a lot of fat and feels wet even when i put it infront of a fan... so i put it in a dessicant chamber... i dont want to try it before i get a response...

how can i clean or wash this freebase without re A/B?
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