Paradox
©
Fisana

Jump to content


Photo
- - - - -

Freeze precipitation question


  • Please log in to reply
22 replies to this topic

#1 tailsmcsnails

tailsmcsnails

    "DOOR"

  • Black VIP
  • 452 posts

Donator


Awards Bar:

Posted 15 February 2017 - 05:29 AM

This puzzles me:

 

In ACRB a/b extraction, I'm told to put the final naptha pulls into a dish, and let them air-evaporate decreasing the naptha volume by 50%.  I understand why you'd do this.

 

Then, when you put the partly-evaporated DMT-laden naptha in the freezer, we're told to cover it tightly.

 

I don't understand why.

 

Help me understand, wise Mycotopians.

 

:-)

 



#2 JanSteen

JanSteen

    Mycophage

  • Free Member
  • 137 posts

Awards Bar:

Posted 15 February 2017 - 09:51 AM

High temperatures cause atoms and molecules to bump into each other harder and faster.
As a result, evaporation at higher temperatures causes more damage to whatever is in the solvent. Lower temperatures also prevent oxidation to some(!) extent.
In freezer conditions, water vapour is removed from the air because it freezes. That way water from the air has less interference with your molecules, it keeps your extract drier compared to regular air.
Also, the conditions are more stable of course.

I'm clueless about DMT extractions, but those are some examples of why one would do stuff in subzero temperatures.

#3 Defiance

Defiance

    Trainee

  • OG VIP
  • 1,385 posts

Posted 15 February 2017 - 11:34 AM

Solubility decreases with temperature as a general rule.

 

As the solvent gets colder, it holds less DMT.



#4 Final

Final

    Mycophiliac

  • Free Member
  • 75 posts

Posted 15 February 2017 - 12:51 PM

Dont bother , just a waste of solvent.  just use less solvent with each pull, doing that u can freeze precipe in as little as 2-3 hrs per pull.   

use just enough to barely cover the bark soup. and tilt the jar in order to suck up to put in the freeze precipe dish. 

 

 

if u dont mind me asking, 

 

what tek are you using ?

 

what is/was your yield ? 

acrb can easily get 2.5% yield if the cells were lysed enough .


  • tailsmcsnails likes this

#5 tailsmcsnails

tailsmcsnails

    "DOOR"

  • Black VIP
  • 452 posts

Donator


Awards Bar:

Posted 15 February 2017 - 06:25 PM

Dont bother , just a waste of solvent.  just use less solvent with each pull, doing that u can freeze precipe in as little as 2-3 hrs per pull.   

use just enough to barely cover the bark soup. and tilt the jar in order to suck up to put in the freeze precipe dish. 

 

 

if u dont mind me asking, 

 

what tek are you using ?

 

what is/was your yield ? 

acrb can easily get 2.5% yield if the cells were lysed enough .

Yeah I've worked out that less is more when it comes to the amount of naptha used.

 

I understand how precipitation and crystalisation works, I just don't understand why you'd cover it in the freezer (but not before)- evaporation is evaporation right?

 

From 100g of bark I got at least that 2.5g, we stopped weighing and started smoking but it was HEAPS.

 

The tek I used is more or less this one https://www.dmt-nexu...g=posts&t=64608

 

share everything you know immediately ;-)



#6 tailsmcsnails

tailsmcsnails

    "DOOR"

  • Black VIP
  • 452 posts

Donator


Awards Bar:

Posted 15 February 2017 - 06:33 PM

oops duplicate post


Edited by tailsmcsnails, 15 February 2017 - 06:39 PM.


#7 Defiance

Defiance

    Trainee

  • OG VIP
  • 1,385 posts

Posted 15 February 2017 - 06:33 PM

You just cover it so it won't spill and mess up your food. I has nothing to do with any sort of evaporation or chemistry. Uncovered is fine too.


  • tailsmcsnails likes this

#8 tailsmcsnails

tailsmcsnails

    "DOOR"

  • Black VIP
  • 452 posts

Donator


Awards Bar:

Posted 15 February 2017 - 06:36 PM

You just cover it so it won't spill and mess up your food. I has nothing to do with any sort of evaporation or chemistry. Uncovered is fine too.

 

thank you!  I sort of assumed that was the case, since I have a freezer with nothing but freezing DMT in it I shan't worry about covering it any more.

 

Also may I add that advice to get hold of some pyrex baking trays has changed my life.  Scraping every last morsel out of an assortment of jam jars was not the most fun I've ever had!  


Edited by tailsmcsnails, 15 February 2017 - 06:40 PM.

  • Defiance and CatsAndBats like this

#9 Final

Final

    Mycophiliac

  • Free Member
  • 75 posts

Posted 15 February 2017 - 08:13 PM

 

Dont bother , just a waste of solvent.  just use less solvent with each pull, doing that u can freeze precipe in as little as 2-3 hrs per pull.   

use just enough to barely cover the bark soup. and tilt the jar in order to suck up to put in the freeze precipe dish. 

 

 

if u dont mind me asking, 

 

what tek are you using ?

 

what is/was your yield ? 

acrb can easily get 2.5% yield if the cells were lysed enough .

Yeah I've worked out that less is more when it comes to the amount of naptha used.

 

I understand how precipitation and crystalisation works, I just don't understand why you'd cover it in the freezer (but not before)- evaporation is evaporation right?

 

From 100g of bark I got at least that 2.5g, we stopped weighing and started smoking but it was HEAPS.

 

The tek I used is more or less this one https://www.dmt-nexu...g=posts&t=64608

 

share everything you know immediately ;-)

 

 

please be cautious on ordering lye,  https://www.dmt-nexu...?g=posts&t=1751  @ Mods sry if its advertising but its legit in regards to member safety.

 

you know what your doing 2.5% is excellent the cells were lysed and was good bark , you prolly cooda banged out 2.8 but im guessing felt wastful doing a pull just to get 40 mg ish. 

 

i would say give q21q21 tek a shot. but double the amount of liquid and cook the bark vinegar and purified water for least an hour, bring to boil then lower heat to simmer for remainder of time. 

 

I think people cover it so their freezer doesn't stink of the solvent .

 

imo evap is not needed, rather then say use 2 precip dishes and 5 pulls each dish and wait 24 hrs,  

if u have the space, id say use 5-10 precip dishes 1-2 tiny pulls each and check it every hour, waste a lot less solvent since no evap needed.  

if their is spice floating in the precipe dish, using coffee filters is gr8 way to get them out, but u may los a lil solvent that gets absorbed by the filter paper. 

 

Heating solvent up, for max fire safety, bring water to a simmer or least 140-150f/ 60-65 c, remove from the area with the range, and heat solvent up in the hot water. 



#10 tailsmcsnails

tailsmcsnails

    "DOOR"

  • Black VIP
  • 452 posts

Donator


Awards Bar:

Posted 15 February 2017 - 10:05 PM

 

please be cautious on ordering lye,  https://www.dmt-nexu...?g=posts&t=1751  @ Mods sry if its advertising but its legit in regards to member safety.

 

you know what your doing 2.5% is excellent the cells were lysed and was good bark , you prolly cooda banged out 2.8 but im guessing felt wastful doing a pull just to get 40 mg ish. 

 

i would say give q21q21 tek a shot. but double the amount of liquid and cook the bark vinegar and purified water for least an hour, bring to boil then lower heat to simmer for remainder of time. 

 

I think people cover it so their freezer doesn't stink of the solvent .

 

imo evap is not needed, rather then say use 2 precip dishes and 5 pulls each dish and wait 24 hrs,  

if u have the space, id say use 5-10 precip dishes 1-2 tiny pulls each and check it every hour, waste a lot less solvent since no evap needed.  

if their is spice floating in the precipe dish, using coffee filters is gr8 way to get them out, but u may los a lil solvent that gets absorbed by the filter paper. 

 

Heating solvent up, for max fire safety, bring water to a simmer or least 140-150f/ 60-65 c, remove from the area with the range, and heat solvent up in the hot water. 

 

Thanks I will check out that tek, and the safety warning about lye and heating naptha.  I have learned a lot from following the tek I posted to the letter the first time, then adjusting things like using way less naptha and way more patience and agitation as I started to understand where the DMT was in each step and why.

 

I did actually go back to my first bark soup for a few more extractions- so you may be  right about the 2.8g as it was pretty much snowing DMT.  Even in the final pulls of exhausted soup I was getting enough crystals that I would have called it a success based on my modest expectations before I started!  I just got lazy about weighing it after I realised that there was lots, and scraping it out of jars was a PITA and took all my attention.  This current extraction that is  precipitating right now in nice flat baking dishes, I will weigh properly and report back.

 

I've been thinking about filtering out the floaty crystals but since that naptha gets recycled anyway, I figure it will come out at some stage?

 

Off to check out the q21q21 tek!  Thanks for the chance to chat, I'm a little obsessed at the moment.


Edited by tailsmcsnails, 15 February 2017 - 10:06 PM.


#11 tailsmcsnails

tailsmcsnails

    "DOOR"

  • Black VIP
  • 452 posts

Donator


Awards Bar:

Posted 16 February 2017 - 04:42 AM

OK I got 2.1g of the most beautiful acicular crystals from round one of batch 2. Man I love those Pyrex pans. I went back to the soup tonight with a little more naptha to see if I can get any more.
  • CatsAndBats likes this

#12 Final

Final

    Mycophiliac

  • Free Member
  • 75 posts

Posted 16 February 2017 - 09:03 AM

 

 

please be cautious on ordering lye,  https://www.dmt-nexu...?g=posts&t=1751  @ Mods sry if its advertising but its legit in regards to member safety.

 

you know what your doing 2.5% is excellent the cells were lysed and was good bark , you prolly cooda banged out 2.8 but im guessing felt wastful doing a pull just to get 40 mg ish. 

 

i would say give q21q21 tek a shot. but double the amount of liquid and cook the bark vinegar and purified water for least an hour, bring to boil then lower heat to simmer for remainder of time. 

 

I think people cover it so their freezer doesn't stink of the solvent .

 

imo evap is not needed, rather then say use 2 precip dishes and 5 pulls each dish and wait 24 hrs,  

if u have the space, id say use 5-10 precip dishes 1-2 tiny pulls each and check it every hour, waste a lot less solvent since no evap needed.  

if their is spice floating in the precipe dish, using coffee filters is gr8 way to get them out, but u may los a lil solvent that gets absorbed by the filter paper. 

 

Heating solvent up, for max fire safety, bring water to a simmer or least 140-150f/ 60-65 c, remove from the area with the range, and heat solvent up in the hot water. 

 

Thanks I will check out that tek, and the safety warning about lye and heating naptha.  I have learned a lot from following the tek I posted to the letter the first time, then adjusting things like using way less naptha and way more patience and agitation as I started to understand where the DMT was in each step and why.

 

I did actually go back to my first bark soup for a few more extractions- so you may be  right about the 2.8g as it was pretty much snowing DMT.  Even in the final pulls of exhausted soup I was getting enough crystals that I would have called it a success based on my modest expectations before I started!  I just got lazy about weighing it after I realised that there was lots, and scraping it out of jars was a PITA and took all my attention.  This current extraction that is  precipitating right now in nice flat baking dishes, I will weigh properly and report back.

 

I've been thinking about filtering out the floaty crystals but since that naptha gets recycled anyway, I figure it will come out at some stage?

 

Off to check out the q21q21 tek!  Thanks for the chance to chat, I'm a little obsessed at the moment.

 

 

 

hmm if I understand you correctly.  the floating spice in freeze precip dish,   

 

once u pull the precip dish out of the freezer, if there is a lot of spice floating, np get a glass cup, a coffee filter, and pur the solvent into that, and scrape or gently flick the spice in the coffee filter back into the precip dish. 

 

then lean the dish and have a fan blow air on it, this accelerates evaporation of the naptha and dries the spice very fast . 

 

did i understand you correctly ?

 

i wouldnt be surprised if 3% yield is achievable, its just that after the 2.4-2.5 % mark each pull or 2 might only be like 30-50mg a pull vs your first pulls of being 450mg plus. 



#13 tailsmcsnails

tailsmcsnails

    "DOOR"

  • Black VIP
  • 452 posts

Donator


Awards Bar:

Posted 16 February 2017 - 02:59 PM

please be cautious on ordering lye, https://www.dmt-nexu...?g=posts&t=1751 @ Mods sry if its advertising but its legit in regards to member safety.

you know what your doing 2.5% is excellent the cells were lysed and was good bark , you prolly cooda banged out 2.8 but im guessing felt wastful doing a pull just to get 40 mg ish.

i would say give q21q21 tek a shot. but double the amount of liquid and cook the bark vinegar and purified water for least an hour, bring to boil then lower heat to simmer for remainder of time.

I think people cover it so their freezer doesn't stink of the solvent .

imo evap is not needed, rather then say use 2 precip dishes and 5 pulls each dish and wait 24 hrs,

if u have the space, id say use 5-10 precip dishes 1-2 tiny pulls each and check it every hour, waste a lot less solvent since no evap needed.

if their is spice floating in the precipe dish, using coffee filters is gr8 way to get them out, but u may los a lil solvent that gets absorbed by the filter paper.

Heating solvent up, for max fire safety, bring water to a simmer or least 140-150f/ 60-65 c, remove from the area with the range, and heat solvent up in the hot water.

Thanks I will check out that tek, and the safety warning about lye and heating naptha. I have learned a lot from following the tek I posted to the letter the first time, then adjusting things like using way less naptha and way more patience and agitation as I started to understand where the DMT was in each step and why.

I did actually go back to my first bark soup for a few more extractions- so you may be right about the 2.8g as it was pretty much snowing DMT. Even in the final pulls of exhausted soup I was getting enough crystals that I would have called it a success based on my modest expectations before I started! I just got lazy about weighing it after I realised that there was lots, and scraping it out of jars was a PITA and took all my attention. This current extraction that is precipitating right now in nice flat baking dishes, I will weigh properly and report back.

I've been thinking about filtering out the floaty crystals but since that naptha gets recycled anyway, I figure it will come out at some stage?

Off to check out the q21q21 tek! Thanks for the chance to chat, I'm a little obsessed at the moment.

hmm if I understand you correctly. the floating spice in freeze precip dish,

once u pull the precip dish out of the freezer, if there is a lot of spice floating, np get a glass cup, a coffee filter, and pur the solvent into that, and scrape or gently flick the spice in the coffee filter back into the precip dish.

then lean the dish and have a fan blow air on it, this accelerates evaporation of the naptha and dries the spice very fast .

did i understand you correctly ?

i wouldnt be surprised if 3% yield is achievable, its just that after the 2.4-2.5 % mark each pull or 2 might only be like 30-50mg a pull vs your first pulls of being 450mg plus.
I think you understood me, nothing you said is different to what I've been doing which is good as I wonder sometimes what weird mistakes or misinterpretations I'm making.

there was small but significant yield in last night's pull so that soup ain't finished yet. I'll just put a few ml of naptha thru it every night til it comes up dry, as an experiment.

Edited by tailsmcsnails, 16 February 2017 - 03:00 PM.


#14 scott_1971_h

scott_1971_h

    Mycotopiate

  • VIP
  • 313 posts

Posted 17 February 2017 - 05:29 AM

Has anyone ever tried evaporating solvents under a vacuum? 



#15 CatsAndBats

CatsAndBats

    detective dorkasaurus

  • OG VIP
  • 7,742 posts

Awards Bar:

Posted 17 February 2017 - 09:51 AM

https://mycotopia.ne.../523-ab-vs-stb/

 

just visual fyi



#16 SteampunkScientist

SteampunkScientist

    Distinguished Mad Scientist

  • OG VIP
  • 2,472 posts

Donator


Awards Bar:

Posted 17 February 2017 - 11:28 AM

Okay.  Here is what is going on.
 
Naptha holds both the goodies (spice) and the baddies (yellow crap, various gums, glues, oxidated bits, broken molecules, residues, etc).
 
The bad stuff is, for the most part, more soluble in Naptha than the good spice is.  And the solubility goes up as temperature goes up, but too high temperature, and we start breaking down our precious spice.
 
What we have here is a balancing act.
 
So what we are going to do:
 
1.) After filtering our Naptha we would like to reduce it down in volume to increase the amount of Spice per unit volume of Naptha.  This is called "Creating a saturated Solvent".  We want to have as little Naptha with as much Spice as possible.  We do this by simple evaporation. However, we do not want to evaporate everything because we do not want the bad stuff, nor do we want our Spice falling out of solution in an impure state.  So we reduce our volume of Naptha and Spice solution by 50% which increases the saturation of the Naptha with our Spice and the stuff we do not want.
 
2.) Because of the lucky coincidence that Spice is less soluble in Naptha than the stuff we don't want, we can chill it now and the Spice will make nice white crystals on the side of the jar or floating in the Naptha and we can run this through a coffee filter to get very pure spice crystals.
 
3.) As there will still be goodies in the Naptha after getting those purified crystals out, we want to keep it for future A/B extractions.  However, eventually this Naptha will get dirty, that is, filled with bad stuff.  So now we should just evaporate it all at room temperature. You will be left with a yellow - brown goo.  This goo can be transferred to your Acid portion of the next A/B extraction you do along with the bark and re-extracted with fresh naptha and the whole process begins again.
 
4.) You can do additional washes of the whitish crystals you got through freeze precipitation, to purify it even more.  You put just enough warm Naptha to dissolve your crystals, adding it a drop or two at a time.  Then chill it again.  The Naptha will hold any additional bad stuff, and even more pure crystals will be had.
 
e58fa620ca6560024e692ed14cf2bcb0.jpg


Edited by SteampunkScientist, 17 February 2017 - 11:32 AM.

  • Fresh Brewed, Gnomesayin and tailsmcsnails like this

#17 CatsAndBats

CatsAndBats

    detective dorkasaurus

  • OG VIP
  • 7,742 posts

Awards Bar:

Posted 17 February 2017 - 12:08 PM

I called the steampunk cavalry ^^^


  • SteampunkScientist likes this

#18 Defiance

Defiance

    Trainee

  • OG VIP
  • 1,385 posts

Posted 17 February 2017 - 12:55 PM

3.) As there will still be goodies in the Naptha after getting those purified crystals out, we want to keep it for future A/B extractions.  However, eventually this Naptha will get dirty, that is, filled with bad stuff.  So now we should just evaporate it all at room temperature. You will be left with a yellow - brown goo.  This goo can be transferred to your Acid portion of the next A/B extraction you do along with the bark and re-extracted with fresh naptha and the whole process begins again.

 

You probably shouldn't do that. You're just wasting solvent and dumping all of the junk back in.

 

You can crash clean dirty solvent by putting it in a slush bath in the freezer. All you need is a bunch of ice and salt and some water in a big container. Put the jar of solvent in the bath and leave it in the freezer overnight. The slush gets colder than freezer temps and everything will fall out of solution and yield clean reusable solvent. 

 

You can separate out all the garbage that falls out of dirty solvent by using a density gradient. Put the goo in a test tube with a slight excess of methanol, stir it all up, and then wait. The bright yellow oxide oil will sink to the bottom and form a layer that you can draw off with a syringe. 

 

Try to evaporate as little as possible. Naptha fumes will fuck up your lungs.


Edited by Defiance, 17 February 2017 - 12:58 PM.

  • tailsmcsnails likes this

#19 Final

Final

    Mycophiliac

  • Free Member
  • 75 posts

Posted 17 February 2017 - 02:08 PM

 

3.) As there will still be goodies in the Naptha after getting those purified crystals out, we want to keep it for future A/B extractions.  However, eventually this Naptha will get dirty, that is, filled with bad stuff.  So now we should just evaporate it all at room temperature. You will be left with a yellow - brown goo.  This goo can be transferred to your Acid portion of the next A/B extraction you do along with the bark and re-extracted with fresh naptha and the whole process begins again.

 

You probably shouldn't do that. You're just wasting solvent and dumping all of the junk back in.

 

You can crash clean dirty solvent by putting it in a slush bath in the freezer. All you need is a bunch of ice and salt and some water in a big container. Put the jar of solvent in the bath and leave it in the freezer overnight. The slush gets colder than freezer temps and everything will fall out of solution and yield clean reusable solvent. 

 

You can separate out all the garbage that falls out of dirty solvent by using a density gradient. Put the goo in a test tube with a slight excess of methanol, stir it all up, and then wait. The bright yellow oxide oil will sink to the bottom and form a layer that you can draw off with a syringe. 

 

Try to evaporate as little as possible. Naptha fumes will fuck up your lungs.

 

 

the yellowish stuff is NMT and small amounts of fats,  NMT is semi soluble in Naptha . 

 

fun fact NMT is in human urine wonder if someone knows how to extract it = future of psychonauts, every guy here urinate in a gallon jug n save it, Woman urinate in bucket. we can make so much NMT lol. 

 

https://en.wikipedia...ethyltryptamine



#20 Defiance

Defiance

    Trainee

  • OG VIP
  • 1,385 posts

Posted 17 February 2017 - 02:17 PM

Nah, the yellow oil you get from dirty solvent isn't NMT. It's a viscous liquid at room temps, NMT would be solid. NMT melting point is fairly high for a simple tryptamine at 189F.

It's probably DMT-N-Oxide, since improperly stored crystals will gradually melt into yellow goo.




Like Mycotopia? Become a member today!