Toshido's Lab A/B Tek V1.3

[Toshido]

EDIT: NEW VERSION OF THE TEK IS UNDERWAY WITH LARGE CHANGES, REDUCING THE EXTRACTION TO JUST 10 STEPS (and only taking 2 hours). ALTHOUGH THIS TEK WORKS AND PROVIDED ME WITH A 0.7% YIELD, USE IT AT YOUR OWN DISCRETION AS A NEW VERSION IS IN THE WORKS AND WILL BE UPDATED IN FEB/MARCH.

Link here. Toshido's New Lab TEK

Tek Preface and Intro:

Much like when I cook food (I love to cook) I will sift around other peoples recipes and combine them together while adding my own flare. I did the same thing here in order to fit my wants and needs, as this Tek draws heavily from....

Cybs Hybrid ATB Salt Tek
&
Psilosopher?'s ATB Tek

It also draws loosely from....

Cybs Max Ion Tek
&
Earthwalker's ACRB Tek

EDIT: SOME STEP BY STEP PICTURES MISSING. COMING SOON

Toshido’s Lab A/B TEK V1.3

My Preferred Equipment List:

1000ml Pyrex Erlenmeyer Flask
1000ml Pyrex Beaker
250ml measuring cylinder for solvent
Small mason jar for preheated Solvent
Shot glass for last solvent pull
Pyrex Measuring Cup
Small Stainless Steel Pot
Rectangular Pyrex Dish for Freeze Crystallization
Hot Plate w/ Magnetic Stirring Capabilities and Thermometer
Magnetic Mixing Stirrer
Magnetic Stirrer Retriever
50ml Professional Slim Pipette
1ml or 5ml Eyedropper
Stainless Steel Funnel
PPE (Gloves, Eye Goggles, Face Mask)
Scale
Coffee Filters
Rubber Band (For attaching coffee filter to funnel)
pH Strips
Cling Wrap
Fan
Razor Blade
Small glass container for crystals.

Ingredients:

50 grams powdered MHRB
50 grams NaOH (Sodium Hydroxide aka Lye/Caustic Soda)
700ml Distilled Water
50ml Vinegar
30 grams Non-Iodized Salt
250ml of Bestine (N-Heptane Solvent)

Some notes about hot plates, magnetic stirrers, emulsions and pulls.

Sensor: Whenever you have to remove the sensor in order to remove the beaker or flask, make sure the heating function is turned OFF. If you have your heat set to 55C and you take the sensor out without turning off the heat, it will think your solution is room temperature and continue to heat your solution. So remember, if the sensor needs removed, turn OFF the heat.

Stirrer RPM: In an effort to prevent splashes and unwanted emulsions, you should always begin your stir at 300rpm. For instance, if the Tek calls for 700rpm, set the stirrer to 300rpm and allow it to reach that speed. Once that speed is reached, then you may gradually increase the speed in 100rpm increments until the desired rpm is reached. Steady and slow.

Emulsions: Stirring too vigorously for too long or at a high heat can create unwanted emulsion that will be temperamental to alleviate, or impossible to rectify without returning the base solution back to an acid and then back to a base, which wastes time and materials. Let rest until solvent separates, about 10 min. Depending on the size and shape of your magnetic stir bar, and the model of hotplate you have, you may need to adjust RPMs accordingly.

Pulls: It is inevitable that you will get some of the MHRB solution into the 250ml measuring cylinder. Especially on your final pull, which will be your largest pull. When decanting the solvent from the cylinder to your pyrex dish, you will be able to get the majority of it. However, the very last bit can be transferred to a shot glass so that you can use an eye dropper to get the remaining solvent.

Extraction Guide:

1) Add 50 grams of MHRB into a 1000ml beaker.

2) Add 200ml distilled water and 50ml vinegar to Pyrex measuring cup, then add to stainless steel pot. Heat to 60C/(140F).

3) Pour the acidic solution into the beaker and manually stir. (You can use your magnetic stirrer retriever for this initial stir.) Solution should be around 300ml.

4) Add the magnetic stir bar and put the beaker onto the hot plate. Set the heat to 60C/(140F.) Set the stirrer to 400RPM for a gentle stir.

5) Leave to soak and stir for 1 hour. If the magnetic stirrer fails to spin, agitate it by stirring manually. If the MHRB is finely powdered, you should have no issue.

6) Put 100ml distilled water into a pot and bring to a pre boil. Add 30g of NON-iodized salt and stir until dissolved. Pour the saline solution into the beaker. You should have a little over 400ml solution total in the beaker. Continue to stir for 15 minutes at 400rpm.

7) Turn OFF hot plate and stirrer and REMOVE THE MAGNETIC STIRRER FROM BEAKER with your retriever. Strain, using a coffee filter and funnel, the saline/acid MHRB solution from the beaker into the flask squeezing out as much liquid as possible. Set aside used MHRB for an optional, later extraction. Place the flask on the hotplate. ADD MAGNETIC STIRRER TO FLASK, this can we done by tilting the flask and sliding it in carefully, or using a strong magnet to guide it. Turn hotplate and stirrer back on. pH should be 4. Thoroughly wash and dry the beaker.[/b]

8) Put 200ml of COLD distilled water into the Pyrex measuring cup. You can place the measuring cup with water in the freezer for 5 minutes for a quick cool down.

9) CAUTION: Measure 50 grams of NaOH (Sodium Hydroxide) and slowly add 1/3 of the NaOH to the water at a time, stirring until dissolved. NaOH will generate an exothermic reaction and become hot in a short amount of time. In the event of spills, use vinegar to neutralize.

10) Carefully add the caustic base solution to the flask.
The liquid should turn almost completely black. pH should be 13.

11) Add another 150ml of distilled water to the flask. The total volume should be around 700ml. Turn heat down to 55C/(135F) and allow to heat and stir for 1.5 hours.

12) Turn off stirrer. Pipette 50ml of N-Heptane (Bestine Solvent) into flask. Turn on stirrer to 700rpm for 5 minutes. (Remembering to start at 300 and increase to 700).

13) Let the solution settle and separate for 5 minutes. You should see 2 distinct layers. Once the solution is separated, turn on the stirrer AGAIN for 5 minutes. Again, let settle and allow to separate for 5 minutes.

14) Pipette the solvent from the flask into the 250ml measuring cylinder. With that math, it should be taking you 20 minutes per pull.

15) Repeat steps 12-14 four additional times. (Pipette 50ml solvent to flask > stir for 5 minutes > let separate for 5 min > stir for 5 minutes > let separate for 5 min > pipette solvent to measuring cylinder)

16) Once you have done 5 pulls. You should have used 250ml of solvent at this point, which should now be in the measuring cylinder. Add to the Square Pyrex dish now. (If you pipetted any of the MHRB solution into the cylinder (inevitable and quite alright), transfer to a shot glass, allow to settle, and use an eyedropper to collect the rest of the solvent.)

17) Cover Pyrex dish with cling wrap, then the rubber lid for a double seal. Carefully incubate the pyrex with a thick towel folded around it, and leave in freezer (-6F is ideal) for 24 hours.

18) Take out Pyrex dish and pour off solvent into a mason jar or original solvent container (use coffee filter to catch any crystals if you'd like) to be reused for a later extraction. Tt should look like this. The crystals are DMT, the bulbous spheres are water/oxygen/solvent (left image) that will soon evaporate after decanting the solvent (right image).

19) Place dish against a wall and gently blow a cold fan on it for 20 minutes until all solvent has evaporated. Don't put the fan too close. There should be only crystals left and product should smell like a flowery new pair of shoes.

20). Using a razor blade, scrape crystals onto a piece of folded paper and let dry completely. Yield should be somewhere around 1-2% (0.5g to 1.0g depending on efficiency of extraction.) Add crystals to a small lidded glass container.

Total Tek Time: 6 Hours (Including step preparation)
Total Freeze Time: 24 Hours

Disposal of used ingredients:
Lye and plant material can be flushed away (bathtub or shower is a great place) as lye is primarily used as a drain cleaner. However, you should add some vinegar to the base solutions to neutralize, and have running water going down the drain as you pour it out slowly. Solvents can be evaporated if done safely, or simply stored in their original containers and sealed, away from heat sources.

Re-X Guide Coming Soon....

End of Tek! Here are some up close pictures of these crystals, which from a bird's eye view look like crystal crustacean fairies. The camera I used is a Canon 60D with a 100mm Macro Lens , a tube extender, and a snap on Raynox Macro Magnfier. Unfortunately, the focal length is down to the millimeter/micron so I couldn't get the best photos.

 

[f1]

I've never done a extraction but I enjoyed reading this and will keep an eye on this thread for developments :thumb_up:

Looking forward to seeing some phots and videos and seeing what members chime in on your tech / process etc.

Have a good one 8)

 

[Hyper Turtle]

-Do my measurements for liquid milliliters and solid grams measure up, I may not have accounted for evaporation/adding water.
-Need notes on storing used solvent, in this case Heptane, but may be worth knowing how to store Naphtha as well because of different flash points.
-Are my steps on the pull methods redundant or inefficient? Should I be crystalizing everything at once as my Tek states in Step 20 or should I be crystalizing each pull separately? ANSWER FROM Homo Trypens: COMBINING IS FINE
-Am I using too much NaOH? I've heard mixed reports of 1:1 grams MHRB to NaOH, while others have stated it's more close to 5:3. I can only assume you would need less NaOH if you are doing an STB (Straight to Base) Tek for obvious reasons, but would like to clarify.
-After pouring off the heptane, is turning the Pyrex dish upside down for a final dripping off of the heptane going to lose precious crystals that gets reabsorbed into the dripping solvent?
-I see some people say ATB and some say A/B, which is it? Or does it matter?

- The volumes and weights sound plausible to me. Been a while since my last extraction though.
- I store my used solvents in the containers they came in. I try to make sure there's no water drops whatsoever if they're metal - i had a leak of d-limonene once, that wasn't too fun... Would love to learn a better way myself!
- You should probably do steps 2-7 at least 2-3 times, to make sure you get all the DMT from the bark. You can then reduce the combined "teas" if it's too much volume. I don't know whether it matters when you add the salt, and if so, whether you should add it before straining or after.
- You might be able to get away with less. It's not a problem to use an excess though, as long as you avoid the soup getting all jelly or soapy.
- I like to put the upside down dish back into the freezer for this, to avoid this potential problem
- I call it A/B when filtering out the bark, ATB when i use acid but leave the bark in, and STB when i leave the bark in and use no acid.

 

[The Traveler]

Thank you for posting this!


Kind regards,

The Traveler

 

[downwardsfromzero]

It's a wonderfully well-documented process, thanks for sharing.

Now, where are those xtal pics? [edit : very nicely added to the OP now :thumb_up: Great job!]

 

[Hailstorm]

Good job, OP!

Q: What would be the reason to stir the basified mixture for 1.5 hours at a reduced temperature?

...Here are my $0.02s:

1. If you specify rpm values, mention the length of the stir bar.
2. I do not think it hurts, but I no longer bother adding NaCl. The solubility of DMT in alkaline water, compared to organic solvents, already seems low enough. There should be enough ionic strength and not much room for DMT molecules once you add plenty of sodium hydroxide.
3. Adding NaOH is conveniently done in an ice bath: the flask is magnetically stirred while sitting in a dish filled with water and ice. The ice bath keeps the temperature low and saves time.
4. If the heptane-water mixture is kept hot (~70 °C) while vortexed, you will need much less solvent. Additionally, during the hot extraction you will see heptane starting to cloud right inside your pipette, giving you a nice visual cue that there is still enough DMT to extract.
5. There is some value in hot solvent evaporation before freeze precipitation. It does not improve the yield much, but does make crystallization proceed faster.

 

[Toshido]

Good job, OP!

Q: What would be the reason to stir the basified mixture for 1.5 hours at a reduced temperature?

...Here are my $0.02s:

1. If you specify rpm values, mention the length of the stir bar.
2. I do not think it hurts, but I no longer bother adding NaCl. The solubility of DMT in alkaline water, compared to organic solvents, already seems low enough. There should be enough ionic strength and not much room for DMT molecules once you add plenty of sodium hydroxide.
3. Adding NaOH is conveniently done in an ice bath: the flask is magnetically stirred while sitting in a dish filled with water and ice. The ice bath keeps the temperature low and saves time.
4. If the heptane-water mixture is kept hot (~70 °C) while vortexed, you will need much less solvent. Additionally, during the hot extraction you will see heptane starting to cloud right inside your pipette, giving you a nice visual cue that there is still enough DMT to extract.
5. There is some value in hot solvent evaporation before freeze precipitation. It does not improve the yield much, but does make crystallization proceed faster.

Step 9 of Philosopher?s Tek mentioned turning the heat down, I have no idea why though.

Thank you, Hailstorm.

1.You're right, I should specify that, thanks for the tip.
2. So you're saying the acid and salt mixture is sufficient and there is no need to basify with anything? I've never heard that before.
3. I'll remember the ice bath for next time, I can see that saving time.
4. Heptane/Water mixture? I can understand less solvent with the vortex, but the flask is so wide at the bottom/mid section that the layer of solvent is too thin to do a pull!
5. Hot solvent evap? You mean letting it evap until it is room temperature before adding to freezer?

 

[wattlez]

I assume he means you don't need to add salt as the lye alone is sufficient, the salt helps "force" out the alkaloids in theory.

Nice tek and very well written- I like seeing a fire extinguisher in the picture too

Also gave me some inspiration to pipette my solvent pulls in a measuring cylinder and just pipette out any base soup that made its way there before I begin evap/freeze precipitation, so thanks for that!

Have you tried at higher temperatures when doing your acid stir or pulls?

 

[artificer]

I like this widderic! I have question tho about:

7) Turn OFF hot plate and stirrer and REMOVE THE MAGNETIC STIRRER FROM BEAKER with your retriever. Strain, using a coffee filter and funnel, the saline/acid MHRB solution from the beaker into the flask squeezing out as much liquid as possible.

I've tried teks calling to filter and re-filter by various means (coffee filter, buchner funnel with Celite 545 etc), and then I've tried BLAB tek that does not involve any filtering - IME the filtration is the most arduous task of any tek because the fine MHRB turns into impenetrable rubber mat as it cools passing through filter (tannins?), and I'm not even sure what is or is not gained by filtering. One time I placed the stirred, acidic, unfiltered MHRB soup in refrigerator overnight and filtered the next day, the filtration went MUCH better, but I'm not sure what it might've done to yield.

Anyway, I imagine "squeezing out as much liquid as possible" with coffee filter is a delicate dance to get what you can without ripping the coffee filter. OP could you elaborate on your experience with just this step?

Anyone care to comment on filtration? Is it even needed? Is anything lost by refrigerating/precipitating the tannins before filtration? Am I alone in being frustrated with the most challenging/labor intensive step in these teks (generally) having least amount of information? Does MHRB powder filter easily for others and is it just my bad experience?

 

[Voidmatrix]

2. So you're saying the acid and salt mixture is sufficient and there is no need to basify with anything? I've never heard that before.

I think they're stating that they don't add salt because there should already be enough ionic strength.

5. Hot solvent evap? You mean letting it evap until it is room temperature before adding to freezer?

Though, I put my pulls in the fridge in between pulls and do a cold evap until it reaches room temp. Then allow to evaporate down about 40% (really, until the solvent is saturated), then place in the freezer for freeze precipitation.

Wonderful job on this tek :thumbs up

One love

 

[Toshido]

Have you tried at higher temperatures when doing your acid stir or pulls?

This was my first ever extraction so I have NOT.

Anyway, I imagine "squeezing out as much liquid as possible" with coffee filter is a delicate dance to get what you can without ripping the coffee filter. OP could you elaborate on your experience with just this step?

What I did was place the coffee filter in my stainless steel funnel, and then I surrounded the wet MHRB that wouldn't go through the filter with 2 more coffee filters. Essentially it was a sphere of MHRB surrounded by coffee filters that I could then HAND squeeze while wearing PPE to get 99 percent of the moisture out. I have no idea how it effects yield, I would imagine you get less yield, but I think the purpose is to have less of a substrate for a soup, and more of a soup for a soup. It made it easier on the magnetic stirrer too.

Though, I put my pulls in the fridge in between pulls and do a cold evap until it reaches room temp. Then allow to evaporate down about 40% (really, until the solvent is saturated), then place in the freezer for freeze precipitation.

I've seen others do that, until the naphtha or heptane is almost milky yellow before moving to the freeze precipitation phase.

Indeed there are a lot of things to experiment with here, and I'm excited to do so.

 

[Hailstorm]

I think they're stating that they don't add salt because there should already be enough ionic strength.

Yes, exactly. Water with sodium hydroxide and sodium acetate seems to have sufficient ionic strength even without extra sodium chloride. DMT freebase has very low solubility in high-pH water and partitions well into the organic layer. I have not yet been able to observe a higher yield with NaCl vs. just doing enough hot pulls. Maybe I failed to add enough salt, but it did not "salt out" anything measurable for me. YMMV.

Step 9 of Philosopher?s Tek mentioned turning the heat down, I have no idea why though.

The puzzling part is not turning the heat down – that makes a lot of sense. What is unclear is why one would continue to stir the basified mixture, for hours no less. Basification happens very quickly – once you see the liquid turn black, you can be rest assured your DMT is deprotonated and ready for immediate extraction with an NPS. If anything, prolonged stirring would invite some oxidative DMT degradation and yield loss. I hope our friendly chemists can chime in here, since I could be missing something here.

5. Hot solvent evap? You mean letting it evap until it is room temperature before adding to freezer?

A lot of people evap it at room temperature, which is the classic way. I lack patience, so I reduce it in an evaporation dish that is heated on a hotplate, with a small USB fan next to it blowing up (i.e. diagonally, up and sideways) to create a bit of "vacuum" over the solvent, avoid blowing dust into it, and speed up evaporation. Then I decant the hot solution into a small Erlenmeyer flask, stopper it, wrap it in some cloth or aluminum foil to insulate it, and let it cool down to room temperature - very slowly, to obtain large white crystals. I then move it to a refrigerator for a few hours, and finally it spends the night in the medical freezer. The slower you cool the mixture down, the less impurities will be trapped in the crystals.

Hot evaporation can improve the yield since you start the crystallization process with the DMT dissolved in as little solvent as possible. However, the difference in yield is likely negligible, so it mostly just saves time.

4. Heptane/Water mixture? I can understand less solvent with the vortex, but the flask is so wide at the bottom/mid section that the layer of solvent is too thin to do a pull!

You have some water in the flask, and some heptane floating above it. The diameter is smaller towards the top, making it convenient to pipette the top (heptane) layer out. In a way, the flask-pipette system becomes an upside-down "separatory funnel". That part, I think, we understand the same.

What I meant to say was this:

1) vortex (i.e. stir/agitate well) the two layers to maximize the area of contact between water and heptane and allow as much DMT to partition (migrate) into the organic phase as possible
2) more importantly, the flask should be heated while stirred, the liquids inside should be at ~70-75 °C (avoid boiling though) – hot heptane extracts a lot more DMT, and the less solvent you have to use, the better.

 

[Toshido]

Yes, exactly. Water with sodium hydroxide and sodium acetate seems to have sufficient ionic strength even without extra sodium chloride. DMT freebase has very low solubility in high-pH water and partitions well into the organic layer. I have not yet been able to observe a higher yield with NaCl vs. just doing enough hot pulls. Maybe I failed to add enough salt, but it did not "salt out" anything measurable for me. YMMV.

Oh my, so if I we're to skip this salt phase, all I would need is the vinegar at that point? Would using citric acid or hydrochloric acid increase yield? Or is the point to just get pH to 4?

Basification happens very quickly – once you see the liquid turn black, you can be rest assured your DMT is deprotonated and ready for immediate extraction with an NPS. If anything, prolonged stirring would invite some oxidative DMT degradation and yield loss. I hope our friendly chemists can chime in here, since I could be missing something here.

If this is true, which it sure makes sense that it would be true, then I'd be happy to eliminate another step. When I added the base to the acid solution, I could see a shimmering white substance leap out and then immediately disappear before the whole thing turned black, so obviously there was some reaction there.

However, step 5 of Cybs Tek states...

Shake the mixture up; it should go very dark...almost black.
Put the bottle in a heat bath as before (Warm/cool cycling) and soak for at least 1-2 hours, re-heating the pan if necessary.
Shake the mixture occasionally to prevent settling.

So what's up with that? Is he wrong to be doing that? Can I eliminate this step and go straight to pulling?

A lot of people evap it at room temperature, which is the classic way. I lack patience, so I reduce it in an evaporation dish that is heated on a hotplate, with a small USB fan next to it blowing up (i.e. diagonally, up and sideways) to create a bit of "vacuum" over the solvent, avoid blowing dust into it, and speed up evaporation. Then I decant the hot solution into a small Erlenmeyer flask, stopper it, wrap it in some cloth or aluminum foil to insulate it, and let it cool down to room temperature - very slowly, to obtain large white crystals. I then move it to a refrigerator for a few hours, and finally it spends the night in the medical freezer. The slower you cool the mixture down, the less impurities will be trapped in the crystals.

Wowza, sounds like something I'd like to master. Adding an Evap Dish to my lab list. I'm confused though. You said you decant the solution from the evap dish to a small Erlenmeyer flask to cool slowly for large crystals, and then to the fridge, and then to the freezer but.... how are you getting the crystals out of the Erlenmeyer flask?

You have some water in the flask, and some heptane floating above it. The diameter is smaller towards the top, making it convenient to pipette the top (heptane) layer out. In a way, the flask-pipette system becomes an upside-down "separatory funnel". That part, I think, we understand the same.

I've already added a separatory funnel to my lab, so I can just eliminate pipetting solvent into the evaporation dish from now on? But will probably pipette from flask to cylinder, and then pour from cylinder to sep funnel to keep the mess down.

2) more importantly, the flask should be heated while stirred, the liquids inside should be at ~70-75 °C (avoid boiling though) – hot heptane extracts a lot more DMT, and the less solvent you have to use, the better.

Ok... I was doing 60C for the acidic solution, and then 55C for the basic solution, should I be having both them hotter? I got those temperatures from Philosopher?'s Tek

Thanks so much for your input Hailstorm.

I have spoken with benzyme, and he has confirmed that I can go straight to pulling after basification and adding preheated solvent, and that my base solution should be allowed to cool to room temp before adding the preheated solvent so that the dmt transfers more efficiently. But it was during chat and I may have heard him wrong or there may have simply been some miscommunication as to what I was asking.

 

[Hailstorm]

Oh my, so if I we're to skip this salt phase, all I would need is the vinegar at that point?

Yes, and then NaOH or KOH at the basification stage. But please check if the yield is indeed the same or close.

Would using citric acid or hydrochloric acid increase yield? Or is the point to just get pH to 4?

Acidification may help lyse the cells to get DMT out. Apart from that, it makes DMT (acetate) soluble in water, so if you then filter water-insoluble gunk out it serves as an additional purification step. At pH = 4.68 (i.e. 8.68 - 3) approximately 99.9% (i.e. 1 - 10³ ) of the DMT will be protonated and water-soluble, so it makes little sense to go much below ~4.

The yield should be the same with citric or hydrochloric acid. However, there is a paper that shows that tryptophan undergoes substantial degradation upon standing in hydrochloric acid. I am not aware of any DMT-specific experiments, and hydrochloric acid definitely works, but since DMT and tryptophan are structurally similar, I would personally stay away from hydrochloric acid if acetic acid is available. The only neat thing about HCl is that it forms the old good NaCl after you basify with NaOH.

When I added the base to the acid solution, I could see a shimmering white substance leap out and then immediately disappear before the whole thing turned black, so obviously there was some reaction there.

That was DMT. As the base dissolves in the water it forms local regions of high pH. In those regions DMT precipitates as the white "cloud" you saw and then disperses if the amount of water is substantial. If, however, you dissolve some DMT in a small amount of vinegar and basify it right there, the white substance (DMT) will not disappear and you will be able to filter it out of the water with no NPS at all.

So what's up with that? Is he wrong to be doing that? Can I eliminate this step and go straight to pulling?

Does your tek include filtering the acidified mixture? I like doing so to get rid of all the dust and gunk, avoid emulsions, etc. Basification then happens almost instantly.

If, however, you basify and extract an unfiltered suspension then I guess the point of stirring it for 1-2 hours is to lyse the cells even more and get even more DMT out? I have no idea if that helps. If you want to conduct some experiments, make sure you only change 1 thing at a time.

how are you getting the crystals out of the Erlenmeyer flask?

You can extract solids from an Erlenmeyer flask using a silicone or stainless steel mini-spatula – watch some Youtube videos on recrystallization. But it is not really important – if you prefer dishes and scraping and fan, that works fine. If you crystallize in a ground joint Erlenmeyer flask you can decant the solvent and use a vacuum pump to dry the crystals inside the flask without exposing them to air, so they stay perfectly white without any signs of yellow oily DMT N-oxide covering them.

I've already added a separatory funnel to my lab, so I can just eliminate pipetting solvent into the evaporation dish from now on?

No, not with hot extractions. You don't want to be shaking a hot separatory funnel with caustic and flammable liquids inside. I recommend heating and stirring in the flask on a hotplate and pipetting the top layer out, as you are already doing – it is convenient and safe. If, however, you use a non-heptane solvent to extract DMT, like DCM or amyl acetate, then the temperature is not an issue and a separatory funnel becomes handy indeed.

Ok... I was doing 60C for the acidic solution, and then 55C for the basic solution, should I be having both them hotter?

Not necessarily. The hotter the water-NPS mixture is, the more DMT you extract per pull. However, the hotter it is, the faster DMT degrades. DMT salts are far more stable to oxidative degradation than DMT freebase, so whatever you do, try to avoid heating DMT freebase too much and/or for too long. Heating tbe system to 70-75 °C for a minute and then pulling is fine.

I have spoken with benzyme, and he has confirmed that I can go straight to pulling after basification and adding preheated solvent, and that my base solution should be allowed to cool to room temp before adding the preheated solvent so that the dmt transfers more efficiently. Makes sense.

Adding pre-heated solvent to cool water is something I disagree with. The NPS immediately cools down upon mixing with water, as water has far more thermal capacity – you can measure the temperature yourself. Please see this thread here: Dont Heat Naphtha, Heat your Soup! - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus

 

[Toshido]

it makes little sense to go much below ~4.

Thanks, I'll make sure to keep the pH of the acidic solution between 4.5-4.

Does your tek include filtering the acidified mixture?

This makes sense now. In my tek, yes I filter. His tek did not, so that's probably why he decided to stew it for longer... and oversight on my part for not realizing that. Thank you.

You don't want to be shaking a hot separatory funnel with caustic and flammable liquids inside.

I was going to say... by the time I do 5 pulls (the solvent in my cylinder is going to be close to room temp, and once added to the sep funnel, should not be that hot, but I wouldn't need to shake the sep funnel either way as it will separate on it's own and I can decant from the bottom?

The hotter the water-NPS mixture is, the more DMT you extract per pull. Heating the system to 70-75 °C for a minute and then pulling is fine.

Ok so, heating is ok up to 70C as long as it's not for a long time. My Tek requires that you mix the solution and solvent for 5 minutes, let settle for 5 minutes, then mix and settle 4 more times for a total of 5 times, total of 50 minutes, then pull, then repeat ALL OF THAT 4 more times. So that's 5 hours for 5 pulls while heating at 55c. Sounds like it's overkill to me. And with that you said about heat breaking down dmt, that's probably why my yield was .35g from 50g of MHRB. Too much heat for too long.

Adding pre-heated solvent to cool water is something I disagree with. The NPS immediately cools down upon mixing with water, as water has far more thermal capacity. Please search a thread here, called "do not heat your NPS, heat water" or something.

Yeah in my head I was thinking... wouldn't the room temp solution in the flask immediately cool down the solvent? I'm so confused about all of the contradictions in the many teks I have read. I'll take a look at that thread now. Can't find it, tried multiple search variations.

 

[Hailstorm]

I have updated the above post with the link to the thread.

Regarding the separatory funnel – it will be hard to prevent the liquids from cooling down quickly. Run an experiment: heat some water to 75 °C, pour it into your separatory funnel, shake it for a minute, drain, and quickly measure the temperature. I bet it will be in the 40s.

It is also way too dangerous. Even professionals have had countless accidents with separatory funnels. It may slip out of your hands. The glass may have a defect. You may hit something when you shake. You may forget to close the stopcock. You may forget to vent and the stopper will fly out. You may decide to vent and it will spray your eyes with hot lye. Now, you may be a super careful person who never gets tired, distracted, who never has a bad day. But your followers are not you – since they are reading a tek, it is safe to assume they are not experienced. For harm reduction, please consider sticking to something as safe as a magnetic hotplate stirrer. And even with that, remind people not to stopper the flask tight - the pressure will build up, the boiling point will increase causing the liquids to superheat, the stopper will eventually fly out, the pressure will drop, the water and heptane will instantaneously boil and you will have a caustic, flammable eruption to deal with.

On heat degrading DMT – while that certainly happens, a more frequent case of low yields is something else – like bad bark, not brewing in the acid long enough, not basifying to the right pH, not performing enough pulls and/or not keeping the mixture hot for the NPS to work, not reducing the combined extracts, not giving the crystals enough time to grow in the freezer, etc. Just experiment, and only change 1 variable at a time.

 

[Hailstorm]

Ok so, heating is ok up to 70C as long as it's not for a long time. My Tek requires that you mix the solution and solvent for 5 minutes, let settle for 5 minutes, then mix and settle 4 more times for a total of 5 times, total of 50 minutes, then pull, then repeat ALL OF THAT 4 more times. So that's 5 hours for 5 pulls while heating at 55c. Sounds like it's overkill to me.

Yes, a 5-hour extraction is a major overkill.

Once the liquid is sufficiently basic (pH > 12) and the temperature has stabilized above 70 °C, create a turbulent vortex for a minute, then give the layers a minute to fully separate. Pipette the top layer out, keeping the tip of the pipette away from the water and glass walls that water droplets stick to. If the NPS becomes cloudy in the pipette, it is a good sign you (still) have DMT there. You can also use a powerful 365 nm UV light to see the extract glow.

Keep stirring and pulling until the liquid in the pipette no longer turns cloudy even after a few seconds – the point of diminishing returns. The whole process should not require more than half an hour.

At the end, if you suspect you have picked up some water, you may want to dehydrate the hot combined extract by stirring it with some potassium carbonate (optional), reduce its volume (recommended), and give DMT enough time to crystallize out.

 

[downwardsfromzero]

I have updated the above post with the link to the thread.

Regarding the separatory funnel – it will be hard to prevent the liquids from cooling down quickly. Run an experiment: heat some water to 75 °C, pour it into your separatory funnel, shake it for a minute, drain, and quickly measure the temperature. I bet it will be in the 40s.

It is also way too dangerous. Even professionals have had countless accidents with separatory funnels. It may slip out of your hands. The glass may have a defect. You may hit something when you shake. You may forget to close the stopcock. You may forget to vent and the stopper will fly out. You may decide to vent and it will spray your eyes with hot lye. Now, you may be a super careful person who never gets tired, distracted, who never has a bad day. But your followers are not you – since they are reading a tek, it is safe to assume they are not experienced. For harm reduction, please consider sticking to something as safe as a magnetic hotplate stirrer. And even with that, remind people not to stopper the flask tight - the pressure will build up, the boiling point will increase causing the liquids to superheat, the stopper will eventually fly out, the pressure will drop, the water and heptane will instantaneously boil and you will have a caustic, flammable eruption to deal with.

On heat degrading DMT – while that certainly happens, a more frequent case of low yields is something else – like bad bark, not brewing in the acid long enough, not basifying to the right pH, not performing enough pulls and/or not keeping the mixture hot for the NPS to work, not reducing the combined extracts, not giving the crystals enough time to grow in the freezer, etc. Just experiment, and only change 1 variable at a time.

Excellent harm reduction post - thank you for this :thumb_up:

Please search a thread here, called "do not heat your NPS, heat water" or something.

It's this thread: Dont Heat Naphtha, Heat your Soup!

Yes, a 5-hour extraction is a major overkill.

I always wondered why people put ridiculously long times for NPS extractions - days or weeks, even. Perhaps it was simply to put off the n00bs? Or is it maybe an echo of making tinctures with plant material?
[EDIT: here's an example of that kind of thing, in a critique of "QT's tek"]

- "Shake Jar B, 4 times a day, for 1 week". There is NO need for one week rumba shaking.

 

[Toshido]

I have updated the above post with the link to the thread.

Regarding the separatory funnel – it will be hard to prevent the liquids from cooling down quickly. Run an experiment: heat some water to 75 °C, pour it into your separatory funnel, shake it for a minute, drain, and quickly measure the temperature. I bet it will be in the 40s.

It is also way too dangerous. Even professionals have had countless accidents with separatory funnels. It may slip out of your hands. The glass may have a defect. You may hit something when you shake. You may forget to close the stopcock. You may forget to vent and the stopper will fly out. You may decide to vent and it will spray your eyes with hot lye. Now, you may be a super careful person who never gets tired, distracted, who never has a bad day. But your followers are not you – since they are reading a tek, it is safe to assume they are not experienced. For harm reduction, please consider sticking to something as safe as a magnetic hotplate stirrer. And even with that, remind people not to stopper the flask tight - the pressure will build up, the boiling point will increase causing the liquids to superheat, the stopper will eventually fly out, the pressure will drop, the water and heptane will instantaneously boil and you will have a caustic, flammable eruption to deal with.

I can't tell you how thankful I am for this disclaimer. It really opened my eyes. I certainly would never implement any techniques that I have little to zero knowledge on, which is why I am making my intentions known on this thread. I have not and will not test any methods without sufficient council first, but I DO thank you for reminding me that this is a tek that others will read and how foolish it would be of me to implement a dangerous and unnecessary step. Much thanks.

I read the thread about heating naphtha and it makes so much sense. It was cool to see it broken down on the formula to see how much temperate difference there was from adding heated naphtha to room temp soup vs adding room temp naphtha to heated water.

As for a stopper on a flask. I have been advised that a stopper is simply not needed for the duration of the entire extraction. But if so, I'd love to know why.

On heat degrading DMT – while that certainly happens, a more frequent case of low yields is something else – like bad bark, not brewing in the acid long enough, not basifying to the right pH, not performing enough pulls and/or not keeping the mixture hot for the NPS to work, not reducing the combined extracts, not giving the crystals enough time to grow in the freezer, etc. Just experiment, and only change 1 variable at a time.

Ok got it, so heat degradation is the least of my worries compared to the acidic phase, pH levels, pulls, etc.

Yes, a 5-hour extraction is a major overkill.

Once the liquid is sufficiently basic (pH > 12) and the temperature has stabilized above 70 °C, create a turbulent vortex for a minute, then give the layers a minute to fully separate. Pipette the top layer out, keeping the tip of the pipette away from the water and glass walls that water droplets stick to. If the NPS becomes cloudy in the pipette, it is a good sign you (still) have DMT there. You can also use a powerful 365 nm UV light to see the extract glow.

Keep stirring and pulling until the liquid in the pipette no longer turns cloudy even after a few seconds – the point of diminishing returns. The whole process should not require more than half an hour.

Good to know I can save a substantial amount of time here. When you say cloudy, do you mean the heptane appearing yellow instead of clear?

At the end, if you suspect you have picked up some water, you may want to dehydrate the hot combined extract by stirring it with some potassium carbonate (optional), reduce its volume (recommended), and give DMT enough time to crystallize out.

So the potassium carbonate soaks up what little water is left, what ends up happening to the potassium carbonate then? Does it settle to the bottom or does it end up evaporating with the solvent?

What are some ways to speed up the evaporation process (reducing solvent volume). I'm assuming that the less solvent, the more dmt saturated the solution is, thus making crystallization more effective?

One last question about the solvent. Consider that I would let the combined pulls cool (with some water that I accidentally pulled with it) to room temperature and THEN added to the separatory funnel? What's the issue with having the solvent at room temp if it's just going to go straight to crystallization (freeze precip)?

Again, great post, very thankful to be checked with potentially hazardous steps. I may use that step on my own at some point, but will most certainly not be putting that step in a tek.

I always wondered why people put ridiculously long times for NPS extractions - days or weeks, even. Perhaps it was simply to put off the n00bs? Or is it maybe an echo of making tinctures with plant material?
[EDIT: here's an example of that kind of thing, in a critique of "QT's tek"]

AWESOME link. Tons of helpful information for me to keep in mind when updating my tek. Which is why I'm glad it's a long work in progress with experimentation, and a disclaimer that says that very thing. Last thing I want is to have a QT tek that get's laughed over. Super cool how Shaolin took the time to make corrections and try to get Erowid to fix them. Really helpful to the community. I'll be using his care and attention as a guideline for working out the kinks in my own tek.

 

[Hailstorm]

Thanks widderic and downwardsfromzero!

As for a stopper on a flask. I have been advised that a stopper is simply not needed for the duration of the entire extraction. But if so, I'd love to know why.

A stopper is not necessary – it makes the whole ordeal reek less. I normally just place a 60 mm watch glass over the flask – if the pressure builds up enough to lift it, the watch glass will start vibrating and ringing.

When you say cloudy, do you mean the heptane appearing yellow instead of clear?

I mean an opaque, milky-white suspension. The same color that you see when you evaporate enough solvent and DMT crashes out.

What ends up happening to the potassium carbonate then? Does it settle to the bottom or does it end up evaporating with the solvent?

You decant the solvent off the drying agent (or hot-filter it, which requires a bit of technique). Potassium carbonate is completely insoluble in heptane, and good luck evaporating it. ) You can use sodium carbonate, it works about the same. Neither may be necessary.

What are some ways to speed up the evaporation process (reducing solvent volume).

Hot heptane evaporates incredibly fast. But if you still have to speed the process up, use a fan.

I'm assuming that the less solvent, the more dmt saturated the solution is, thus making crystallization more effective?

Yes, higher concentrations make it more likely for DMT molecules undergoing Brownian motion to "find" each other and stick together.

I would let the combined pulls cool (with some water that I accidentally pulled with it) to room temperature and THEN added to the separatory funnel?

If you used a small amount of hot solvent it will be very saturated and DMT will crash out of it at room temperature. You will have solid DMT floating there – so you'd need a gravity filter, not a separatory funnel.