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official extraction help thread

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Hey guys, I need a little help understanding what’s happening during the water wash stage, specifically related to obtusifolia. My extraction method is A/B and my NPS is toluene.

I performed a water wash using 20ml distilled water, a pinch of sodium carbonate and a pinch of salt.

After washing the toluene the water became murky with clear blobs attached to the surface of the beaker and the toluene became cloudy (it was close to clear before the water wash).

I understand the purpose of a water wash but there’s some things that confuse me:

1) Why are there blobs in the water? What are the blobs? Is it DMT? (I get the same looking blobs when using Shellite for freeze precipitation).

2) Why do we basify the water when we are trying to get rid of base contaminants? Won’t adding base potentially contaminate the NPS further?

I always get a bit derailed at this stage of the extraction, primarily because I have a feeling I’m losing a part of the extract in the water wash. Any help would be greatly appreciated :)
 

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Hey CheeseCat

After washing the toluene the water became murky with clear blobs attached to the surface of the beaker and the toluene became cloudy (it was close to clear before the water wash).
The toluene turning cloudy might be because the added water cooled it down reducing the solubility of dmt in it, that's why the water wash is usually done warm to keep the dmt solubility in the NPS high (both the water and NPS are warmed). It could also be that the water became suspended in the toluene if you shook it vigorously.


1) Why are there blobs in the water? What are the blobs? Is it DMT? (I get the same looking blobs when using Shellite for freeze precipitation).
Not sure about the blobs, maybe some thing about water tension, or the NPS causing the galss to become more sticky, or a film counting the blobs. In any case it seems like something that you should resolve as you need full separation to pull the NPS cleanly.


2) Why do we basify the water when we are trying to get rid of base contaminants? Won’t adding base potentially contaminate the NPS further?
Bcz water, even distilled water, becomes acidic as it absorbs CO2 from the air, the pinch of soda carb is to counter that and minimize dmt losses. The amount of soda carb you're putting is miniscule compared to the base soup the NPS was in contact with. So you won't be further contaminating the NPS unless it was ultra clean to begin with. And yes the base water can become suspended in the NPS but would you rather have lye or soda carb in your final product? The water wash minimizes the risks.

You'll find this thread very relevant.
 
Hey CheeseCat


The toluene turning cloudy might be because the added water cooled it down reducing the solubility of dmt in it, that's why the water wash is usually done warm to keep the dmt solubility in the NPS high (both the water and NPS are warmed). It could also be that the water became suspended in the toluene if you shook it vigorously.



Not sure about the blobs, maybe some thing about water tension, or the NPS causing the galss to become more sticky, or a film counting the blobs. In any case it seems like something that you should resolve as you need full separation to pull the NPS cleanly.



Bcz water, even distilled water, becomes acidic as it absorbs CO2 from the air, the pinch of soda carb is to counter that and minimize dmt losses. The amount of soda carb you're putting is miniscule compared to the base soup the NPS was in contact with. So you won't be further contaminating the NPS unless it was ultra clean to begin with. And yes the base water can become suspended in the NPS but would you rather have lye or soda carb in your final product? The water wash minimizes the risks.

You'll find this thread very relevant.
Awesome, thanks @Sakkadelic! That information is incredibly helpful. I'll read through that thread soon :)
 
Hey, here’s a bit of an update @Sakkadelic...

I tried a water wash again but this time heating both the water and the solvent. This prevented the clear blobs forming in the water portion but there were still blobs forming around the glass where the solvent layer was (see photo).

I noted the water was very murky after washing the solvent and I’m skeptical that the solvent I pulled would have this much contaminant suspended in it? Is it possible the water is washing other plant constituents out?

Both the solvent and the water became milky after being in contact with each other (prior they were both clear).

I’d love to know exactly why the water is so murky and if murky is considered normal? ( I used distilled water with added sodium carbonate and salt).

From here, I'll evaporate the solvent and investigate what I have retrieved.
 

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Hey, here’s a bit of an update @Sakkadelic...

I tried a water wash again but this time heating both the water and the solvent. This prevented the clear blobs forming in the water portion but there were still blobs forming around the glass where the solvent layer was (see photo).

I noted the water was very murky after washing the solvent and I’m skeptical that the solvent I pulled would have this much contaminant suspended in it? Is it possible the water is washing other plant constituents out?

Both the solvent and the water became milky after being in contact with each other (prior they were both clear).

I’d love to know exactly why the water is so murky and if murky is considered normal? ( I used distilled water with added sodium carbonate and salt).

From here, I'll evaporate the solvent and investigate what I have retrieved.
Could you try performing a wash just like you're doing on fresh solvent straight from the can? in theory they should stay seperate and nothing should happen, this will indicate whether the cause of murkiness is the dmt and plant material or something else.

I don't recall seeing before salt used in the wash water, so you can also try without the salt. and are you using tap water?

Are you using fresh soda card? As it sits it goes back soda bicarb. Can you check the ph of the water?

A brine or water wash is also used to clean the solvent so you can expect some stuff to move to the water.

These are just some thoughts, I was trying to find pictures of the water wash on the site to compare but couldn't. I don't remember well how my water wash looked like, and I usually pull alomg the emulsion into the wash, so it's dirty anw.
 
The sodium carbonate is probably 3 years old....seems ok though, no clumping. I tested the pH and the colour was a dark blue so I assumed it was all good. The water is ultra distilled bottled water with no impurities.

I’ll give just the toluene a water wash and see what happens, it's a good idea for comparison (thanks!)

The other thought I had was maybe a defat during the acidic stage might help, but I'm not sure 🤔
 
The sodium carbonate is probably 3 years old....seems ok though, no clumping. I tested the pH and the colour was a dark blue so I assumed it was all good. The water is ultra distilled bottled water with no impurities.

I’ll give just the toluene a water wash and see what happens, it's a good idea for comparison (thanks!)

The other thought I had was maybe a defat during the acidic stage might help, but I'm not sure 🤔
You can also do a mini A/B, it's more effective than a water wash. It depends on what your goal is, if it's to remove base contamination then a wash would do, if it's to have a better chance obtaining purer crystalline dmt then a mini A/B.

I just noticed you mentioned working with obtusifolia, isn't it known to contain more plant oils/fats or whatever it is that gets picked up with the dmt?
 
Yeah, obtuse does have a variety of constituents, likely more varied than other species.

Initially I was interested in crystals but I’ve abandoned freeze precipitation because I can’t find quality naphtha/heptane/hexane and unfortunately shellite results in melting crystals that turn into clear blobs after precipitation. I found shellite works fine with mimosa though (perfect crystals that don’t melt when drying) so there must be something in the composition of acacia crystals that favours being goo rather than a crystal.

Tbh, I’m not really a fan of goo as it’s hard to dose accurately and not ideal for storage but unfortunately acacia doesn’t seem to like the final stage of freeze precipitation so consequently I’m striving for a broader extract with toluene. It’s just the water wash stage that's doing my head in a bit.
 
Yeah, obtuse does have a variety of constituents, likely more varied than other species.

Initially I was interested in crystals but I’ve abandoned freeze precipitation because I can’t find quality naphtha/heptane/hexane and unfortunately shellite results in melting crystals that turn into clear blobs after precipitation. I found shellite works fine with mimosa though (perfect crystals that don’t melt when drying) so there must be something in the composition of acacia crystals that favours being goo rather than a crystal.

Tbh, I’m not really a fan of goo as it’s hard to dose accurately and not ideal for storage but unfortunately acacia doesn’t seem to like the final stage of freeze precipitation so consequently I’m striving for a broader extract with toluene. It’s just the water wash stage that's doing my head in a bit.
That maybe explains things, the acacia and broader extract with toluene pulls more stuff that are making the water murkye and possiby the other observations. I think the best simple path to obtain crystals with acacia is a mini A/B. So after the initial pulls (with shellite preferably) wash the pulls with acidic water, moving the dmt back into water, then remove the shellite and base, then pull with fresh shellite and freeze/precip.

Goo is perfect for changa or enhanced leaf, solves the whole issue with handling, storange and dosage.
 
After washing the toluene the water became murky with clear blobs attached to the surface of the beaker and the toluene became cloudy (it was close to clear before the water wash).

here is a video of the addition of a carbonate to a solution of DMT fumarate. any dmt salt would behave the same. does it look familiar? thats DMT milk. If yoiu have an ultrasonic cleaner you can instantly curdle that emulsion right up as the droplets are forced to collide.

toluene in basic conditions is already kind of prone to emulsing, small droplets kind of repel each other, and in this case theyd rather cling to the glass than each other.
the presence of solid particulates amplifies this effect enormously as the droplets cling so hard to small particles they become incapable of contacting each other, resulting in a waxy film you sometimes see between the water and solvent layer in a sep funnel.

water wash is always a pita for me too since my sources are broad-spectrum regardless of if i used selective solvents, and this might just be a thing that gets worse with jungle spice stuff. actually, just washing toluene with water, period, is a pita. try this instead. wash with a 50% brine, so, saturated salt water, its a little important you filter a slurry, made from originally warm-hot water, rather than make an exact solution because as it cools down the least soluble components precipitate first , resulting in very pure sodium chloride brine. 50% is good, but tweak it. theres merit in using a 100% brine since it will suck the solvent dry of moisture, but its also so dense that it repels all solvents like crazy and helps both phases stay seperate. id add your carbonate though while its a slurry to make an alkaline brine, since carbonate will also cause precipitation of things like calcium.

if your organic phase is free of water, it drastically alters how crystals form later on, though toluene itself strips water out when you boil it, via the azeotrope, so its less useful here than say, hexane/naptha.

the presence of residual brine is likely a non-issue, but trace droplets can be caught out just pouring the toluene through a cotton plugged funnel or basically any porous filter.

Lastly, toluene can be contaminated with numerous things, usually sulfur compounds afaik, or leeched plasticizers from the bottle, or liner of the metal tin if in metal tin.

i recommend everyone buy a cheap little essential oils distillation set and start distilling and/or recycling their own solvents if its not lab grade. the smallest amounts of things like dissolved rubber make a world of difference, same as using distilled water vs tap water. look at every otc solvent like its the tap equivalent of that substance.
 

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Ah ok, I’ll definitely give that a go. Does a mini a/b further refine what is in the NPS, leaving behind fats etc? And no need to water wash after the mini a/b?
Yes and yes, if you wait long enough for full seperation and pull carefully, there won't be a need for a water wash, the main function of which is to minimise the risk of base contamination.
 
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