We've Moved! Visit our NEW FORUM to join the latest discussions. This is an archive of our previous conversations...

You can find the login page for the old forum here.
CHATPRIVACYDONATELOGINREGISTER
DMT-Nexus
FAQWIKIHEALTH & SAFETYARTATTITUDEACTIVE TOPICS
Leaving Mini A-B solution overnight? Options
 
DELETED_USER00002
#1 Posted : 10/4/2016 6:38:50 AM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
Hey all I just about finished with my first A-B extraction as described by EW and the 100g tek, I have put my 1L bottle filled with the saturated acid and had just poured in my left over base, unfortunately I won't be able to return to it till tomorrow to do the final clean pulls with Shellite so I had to put the bottle away!

My question is will the solution be ok tomorrow to just pick up where I left off? My plans is to heat it up again in a water bath to bring it to a good temp for the hot solvent to be more effective.

Without actually having done this before, the only thing that I could think of happening is the freebase will have settled and would need some agitation to mix it up again, other than that what else could happen overnight?

 

Explore our global analysis service for precise testing of your extracts and other substances.
 
Jees
#2 Posted : 10/4/2016 9:59:40 AM

DMT-Nexus member


Posts: 4031
Joined: 28-Jun-2012
Last visit: 05-Mar-2024
Some time in base doesn't hurt, no worries.
Just watch out with heating base soup, be careful not to heat it overly. The solvent is gonna warm too and build up pressure.

Settling FB? (if ever).
The movement/agitation you desperately need for the solvent to come in good contact with the base soup will take care of that, no problem.

Happy trials.
 
downwardsfromzero
#3 Posted : 10/4/2016 10:15:42 AM

Boundary condition

ModeratorChemical expert

Posts: 8617
Joined: 30-Aug-2008
Last visit: 16-Mar-2024
Location: square root of minus one
It will be fine. It takes weeks to months for anything to start going wrong. Make sure you keep it somewhere safe.

If only the freebase would settle out overnight, that would make things much simpler!

All that said, your post is rather unclear as to what you've done and what you're leaving. Saturated acid? Left over base poured in? Something doesn't sound quite right to me.




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
DELETED_USER00002
#4 Posted : 10/4/2016 12:00:12 PM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
My bad, I was in a rush to explain things, I'll explain it again to clear it up

After the whole A-B extraction, I put my Pulls into a bottle with 500mL of acidic solution, then mixed for 10-15 mins, the solvent went from slightly cloudy red/pink to almost clear with a slight tint and the acid turned "salty" (like when you dissolve your salt at the beginning and its cloudy) to me this indicates that the DMT migrated across ok. Then I Pipetted out the solvent and put it in a jar, and added my sodium hydroxide solution and it instantly precipitated out as expected, so I gave this a good shake and this is where I have left it, I will probably run through the soup one more time after this clean up to make sure I didn't miss anything, but initial observations look good. All I need to do now is heat up my solvent and do final pulls Smile will post pics up as soon as I can upload them Smile
 
Tryptallmine
#5 Posted : 10/4/2016 12:35:29 PM

DMT-Nexus member


Posts: 287
Joined: 03-Jan-2014
Last visit: 01-Nov-2017
Astro84 wrote:
My bad, I was in a rush to explain things, I'll explain it again to clear it up

After the whole A-B extraction, I put my Pulls into a bottle with 500mL of acidic solution, then mixed for 10-15 mins, the solvent went from slightly cloudy red/pink to almost clear with a slight tint and the acid turned "salty" (like when you dissolve your salt at the beginning and its cloudy) to me this indicates that the DMT migrated across ok. Then I Pipetted out the solvent and put it in a jar, and added my sodium hydroxide solution and it instantly precipitated out as expected, so I gave this a good shake and this is where I have left it, I will probably run through the soup one more time after this clean up to make sure I didn't miss anything, but initial observations look good. All I need to do now is heat up my solvent and do final pulls Smile will post pics up as soon as I can upload them Smile


It won't go anywhere...it'll still be there in the morning.
 
DELETED_USER00002
#6 Posted : 10/4/2016 1:51:39 PM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
So to put it all together here's what I did to get this far!

First up I made 1L of acid solution, 1L of saline solution and 500mL of basic solution following the guidelines of Earthwalker's tek but just approximating the volume of acetic acid to 1/2 cup (which is 120mL) and rounding up the NaOH to 100g for 500mL water (I used de-ionised water for the whole tek) and 80g salt as per EW's tek. I also put 1/2 a large pot of tap water on the stove on high heat to get the water to a simmer.

As I had not yet made a basic stock before I was extra careful and slow to add the NaOH to the water, and I used a Pyrex jug for the heat. Although it was exothermic, it wasn't as reactive as I had assumed (of course this does not mean I will take any less precautions in the future)

With the stock out of the way, I made a slight change to the tek in the first step of adding water then adding acid, instead I added 500mL acid stock to the dry powdered root bark and mixed well (I figure that it's just one less step for the same result) I placed this bottle in the now hot water bath (at this point I turned the flame to its lowest setting) and I left this in here for 90 minutes (swirling and tipping over the bottle to keep the solution moving. this is what I ended up with: you might see below that there was a fatty layer present on top of the acidified solution.


After 90 minutes, I poured my saline solution into the bottle and mixed well:


Leaving the bottle in the water bath to keep the temperature up, I then added 300mL of my Basic solution to the bottle (reserving the last 200mL for the clean up). the solution turned a deep purple/almost Black as expected:


I left this in the bath on low heat for 2 hours, always swirling and turning over to move the material around and occasionally turning off the heat to stop the water boiling.

After 2 hours I removed the bottle from the water bath and placed it on a towel, I turned the flame off and filled a small jar with Shellite 3/4 full and lowered it into the hot water bath with the lid just loose to release pressure, after a minute or two the shellite started to bubble much the same way a glass of champagne releases bubbles in a stream from a glass. Before the shellite started to boil any further I removed it from the water and Pipetted 50mL of it and placed it into the 2L bottle. (It would be worth noting here that if you have a turkey baster you should bring the jar mouth Close to the bottle as when u lift the baster out it will drip and squirt)

Swirling and turning over for up to a minute and opening the lid to release pressure, I placed the bottle back in the water bath and let it separate for 3+ minutes (I didn't look at the clock I just left it for a bit):

Not easy to see but the solvent floated up and sat on top of the soup.

I very carefully Pipetted out as much solvent as I could and squirted it into a clean jar, instantly the Shellite turned milky with a pink hue, obviously there was some base and some plant fats still present which accounted for the discolouration, however this did not concern me as I had still a Clean up to perform.


I did this 4 more times but because the jar wasn't big enough, I filled the soup with whatever solvent was left ( I think about 100mL) and gave it one last decent mix and Pipetted the last pull into the other jar I used to heat the solvent with.


While this was somewhat a lack of preparation on my behalf, it (unwittingly) showed me that there was not much that remained in the soup in terms of alkaloids because the second jar was no where near as cloudy as the first! I essentially, accidentally evaluated the base soup with the final pull.

I poured the remainder of the acid stock into a 1L bottle ( again lack of preparation because I only had a square bottle not a round one but oh well) and added my Pulls


I mixed considerably, popping the lid to release pressure. The issue I had now was, I had a square bottle, so it made it difficult to avoid emulsion, which is what is mentioned to avoid in EW's tek, I had no other option so I just shook vigorously not taking this into consideration. There was little to no emulsion after the bubbles separated and to my delight the layers had exchanged exceptionally well, the solvent was slightly tinted but mostly clear, and the acid was slightly cloudy but slightly tinted which I expected.


I Pipetted out 99% of the solvent and stored it in a jar and then I poured the remainder of my base stock into the bottle

All that is left now is to do a final pull, and I'll update this post tomorrow with the results Smile

I hope this was as good a read as it was to write!
Peace
 
Tryptallmine
#7 Posted : 10/5/2016 12:24:53 AM

DMT-Nexus member


Posts: 287
Joined: 03-Jan-2014
Last visit: 01-Nov-2017
What I find particularly useful to ensure I end up with very clean spice is to do what is effectively a re-x on my collection jar.
You can see that your collection jar has the pink hue because of aqueous phase contamination. If you drop that collection jar into a heat bath for half an hour, it is very effective at removing a considerable amount of the particulate matter.

I'll then decant that solvent once more into a clean beaker to check the colour and follow it up with a Mini A/B to remove any further plant oils. What precipitates out after that is dry white spice that is very easy to scrape up.
 
DELETED_USER00002
#8 Posted : 10/5/2016 1:58:49 AM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
I will more than likely do a further clean if it's necessary, for now, as this is my first ever experience with an A-B extraction, I feel that I have done well to get this far, I will be doing many more and hope to achieve better results! I will aos take into consideration the materials I used in the process and look for a better alternative such as bottles with longer and more narrow necks for Pipetting better and perhaps taking longer to give the alkaloids every chance to migrate into the solvent. I will post some more results soon Smile
 
downwardsfromzero
#9 Posted : 10/5/2016 12:28:02 PM

Boundary condition

ModeratorChemical expert

Posts: 8617
Joined: 30-Aug-2008
Last visit: 16-Mar-2024
Location: square root of minus one
Talking of removing plant oils, that square olive oil bottle still clearly had oil residue in it so you may have made a backward step with that. Give it a good rinse out with some shellite next time!

Good explanation and pictorial, though! Gives me itchy extraction fingers...




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
DELETED_USER00002
#10 Posted : 10/6/2016 9:51:28 AM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
I'm going to inspect my initial results after tomorrow as it is still in the freezer. I'll see what presents itself to me and see if another re-X will clean up further. The oils would definately be contributed to rushed extraction, next time I'll slow it right down and be more careful
 
DELETED_USER00002
#11 Posted : 10/7/2016 12:06:02 AM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
Air drying as we speak
DELETED_USER00002 attached the following image(s):
20161007_100507.jpg (4,712kb) downloaded 214 time(s).
 
Psilosopher?
#12 Posted : 10/7/2016 1:03:36 AM

Don't Panic

Senior Member

Posts: 756
Joined: 28-Dec-2014
Last visit: 01-Oct-2022
Location: Everywhen
Astro84 wrote:
Air drying as we speak


That's a good looking yield. Have fun!
"A common mistake that people make when trying to design something completely foolproof is to underestimate the ingenuity of complete fools."
 
DELETED_USER00002
#13 Posted : 10/7/2016 3:56:52 AM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
From everything that I could scrape I was so happy to discover that my yield was almost at that magic 1%! There was a tiny bit to scrape which may have got me those .02 extra grams and I decided to leave the shellite out somewhere safe to fully evaporate and see what was left, which may even put me a bit over Smile



Overall from first experience, I am one happy nexian!
It's a little sticky as there was some clear tacky substance underneath and I could re-X and get it a bit cleaner, how does it look to you guys n gals?
 
endlessness
#14 Posted : 10/7/2016 12:15:06 PM

DMT-Nexus member

Moderator

Posts: 14191
Joined: 19-Feb-2008
Last visit: 27-Mar-2024
Location: Jungle
Congrats Smile
 
downwardsfromzero
#15 Posted : 10/7/2016 2:37:55 PM

Boundary condition

ModeratorChemical expert

Posts: 8617
Joined: 30-Aug-2008
Last visit: 16-Mar-2024
Location: square root of minus one
Noice. Is that from ACRB?




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
DELETED_USER00002
#16 Posted : 10/7/2016 9:30:20 PM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
ACRB indeed!
 
DELETED_USER00002
#17 Posted : 10/8/2016 5:50:22 AM
DMT-Nexus member


Posts: 161
Joined: 30-Dec-2012
Last visit: 16-Mar-2018
What's the best way to store Spice?
 
endlessness
#18 Posted : 10/8/2016 1:05:07 PM

DMT-Nexus member

Moderator

Posts: 14191
Joined: 19-Feb-2008
Last visit: 27-Mar-2024
Location: Jungle
 
 
Users browsing this forum
Guest

DMT-Nexus theme created by The Traveler
This page was generated in 0.043 seconds.