If for some reason I shouldn't be posting this yet due to my account age or it's wrong place, just lmn and I'll pull it all down.

I've been researching for a while, spent a chunk of cash on materials and 900g of quality MHRB to start with.

Just wanting to put this somewhere for possible review.

Mainly following Noman's tek, with the addition of Salt and some better tools, as well as a sodium carbonate wash.

ANYways, I wanted to outline my basic procedure and results and get any tips on where I might be missing any glaring easy fixes to gain higher yields.

Before I came to the method I most recently used, I experimented comparing the yields of using a beaker/magnetic stirrer versus mason jars and rolling it around. Beaker and magnetic stirrer won hands down.

I also found that processing 40g at most of MHRB at a time per 1000mL beaker seemed to be the best for getting a good vortex when stirring and mixing well, however I may adjust to 50 after reading Cybs hybrid tek and getting the idea of preparing each substance in a water solution and dissolving each then mixing, as opposed to adding one ingredient at a time to the same container.

I also use a slow cooker as a heat bath and it seems to work well.

1. Add 600mL distilled water to 1000mL beaker.

2. Added 45g of ice cream salt. Stirred the fuck out of it. Took forever to dissolve and then some. This is where dissolving each component into it's own amount of water like Cyb's tek suggests will come in handy for me in the future.

3. Slowly dissolve 40g Lye into water a tsp at a time while the magnetic stirrer does its thing. Tested with pH meter to make sure it was over 12, and used IR thermometer, was at 97 degrees F.

4. Add plant matter 1 tbsp at a time to the solution while the stirrer has a good vortex going. Check pH again to make sure still over 12 and temp is still over 95 degrees.

5. Covered with parafilm and let sit for 1 hour. After that hour, made sure it was still over 95 degrees. If it wasn't (it was) I'd have warmed it in my slow cooker I use for a heat bath.

6. Added 37-39mL VM&P Naptha. Did this while the beaker was being stirred with a small vortex.

7. Stirred in intervals of 5 minutes stirring, 10 minutes sitting. Made sure it stayed over 95 degrees F using the heat bath if necessary. Did this for about an hour, so 4 stirs.

8. Pipetted off the top layer of Naptha, put it into a small jelly mason jar, sealed it and put it in the fridge. Used a thin graduated cylinder to get the last bits cleaning by putting the dirty pull into there and letting it separate, running under a warm tap to help bubbles settle. (I tried using a 1000mL separatory funnel, but tbh I found that it was ineffective for super clean pulls, seemed more effective later on when trying to clean some spice from an old tek)

9. Repeated steps 6-8 three or four more times. Covered beakers with parafilm again and set them aside.

10. Waited 24 hours. (I know most teks say 12, but more my home freezer it seems like 24 hours gives me a much better drop out.)

11. I pull the jars from the freezer, scrape the dmt that's stuck to the bottom so it's just floating in the Naptha, then pour the Naptha and dmt into another large mason jar that a coffee filter is fitted over. The coffee filters are then put into a Tupperware I've put filter covered holes in the side of for clean ventilation.

12. Once dry, crystals are scraped into dram vials and weighed.

RESULTS:

I've done three 40g batches like this, one of which I didn't use the salt, and the other two I did to get a good comparison of how the salt affected yields.

B1 (saltless):
Pull 1 - 313mg
Pull 2 - 224mg
Pull 3 - 086mg
Pull 4 - 024mg
Pull 5 - 024mg
Total = 671mg (1.677% Yield)

B1 (salted):
Pull 1 - 430mg
Pull 2 - 180mg
Pull 3 - 078mg
Pull 4 - 022mg ( I spilled a little of this one though tbh)
Pull 5 - ~0mg
Total = 710 (1.775% Yield)

B1 (salted):
Pull 1 - 386mg
Pull 2 - 187mg
Pull 3 - 099mg
Pull 4 - 063mg
Pull 5 - ~0mg
Total = 735mg (1.837% Yield)

The salt definitely made a difference as expected lol.

I can process three beakers at a time efficiently, as the slow cooker holds two beakers so even if I need a heat bath, it's easy to rotate them in and out on their separate intervals.

So I am getting pretty decent yields. None of the dried crystals are gooey or anything but crystals.

I know I'm loosing some yields in the crystallization process. It seems like no matter how much I scare the coffee filters, they still shine like there's some yields stuck in them. I may try evaporation once I have room to let something sit out without worrying about dust/hair, but right now my yields are super clean.

Just wondering if there's any small improvements I can made? Any better supplies to get things moved from one place to another easier? Etcetera.

Thanks!

-Macrohard.

Welcome Macrohard,

So my free thoughts...

1. You may try to use hydroxide for MHRB decomposition, I do it this way :

Put 50g NaOH into 0,25L of distilled water.
Add 50g of powderized MHRB
Mix thoroughly, the more, the better
Let sit for 24 hours. Mix every few hours
Add 0,5L of distilled water, mix thoroughly
Continue with pulling

2. There is no need for stirrer. The best I found are reagent bottles like this one.
Of course, stirrer may work, but they are usually weak and it is difficult to achieve good vortex for larger volumes.

3. Why are you waiting when stirring? I would stirr without breaks

4. I am not using coffee filters. I just take saturated heptane, put it into beaker, so it is 75% full, cover with foil and put into freezer for a day. Then carefully pour off the heptane, so dmt stays in the beaker, turn the beaker over onto a plate and leave it for 30 minutes to acclimatize. Then put it aside with decent fan for about 24h. The crystals are then scraped off by knife in the beaker. 99% of dmt is removed from the beaker, the rest is waiting there for next crystallization.

5. You may consider using toluene for initial extraction and then use back-salting with subsequent heptane re-x. Toluene allows you to get full-spectrum result, it doesn't have to be saturated, so pulls can use much more of it. Usually two pulls are enough.
I would be careful with NaCl though, I had very bad emulsion when combined these two within dmt extration. I am not using NaCl at all and still getting results > 2.7%

That sounds like a lot (about double what I use), especially with a 24hr wait afterwards . Although I imagine the extra base can't hurt. Any reason for this, out of curiosity ?



An excellent recommendation, thanks - I've been struggling with finding the best containers for this and this one is ideal (and the screw cap is PTB which I believe should stand the NPS much better than other plastics).

To add to pete666's recommendation, if you absolutely have to use a coffee filter after freeze precipitation, then reports on this very forum suggest freezing the coffee filter beforehand helps with limiting melt when filtering the crystals (which makes sense) - although I second pete666's method instead of the filter, it works perfectly.

This is just for the material decomposition. NaOH is very strong base and with this concentration helps to break the bark to same degree. Another water is added afterwards so the final ratio before pulling is as usual.



It's not just the PTB cap, it has PTFE gasket too. This one is really worth buying

That sounds like a good idea, actually, thanks; I tended to make my final pulls a few days later than the others, letting the solution sit for this exact reason, but your approach sounds like it would work faster and require less pulls overall.

Fine powderization, strong NaOH soak, toluene as non-polar and multiple shake/settle cycles (3 first pull, 6 or more second pull) is what ensures everything gets out to the last bit. But be aware that this yields orange dmt, so another purification (mini-A/B with heptane re-x ideally) is needed if pure product is desired.

@pete666

Thanks for the all the tips.

1. I thought about letting it sit with the Lye for 24 hours, but tbh was too impatient wanting to get through multiple runs faster and being okay with doing extra pulls instead. I'll add that 24 hour wait on my next batch most likely.

2. How big of a bottle are you using? I'd love to buy a large bottle that can hold like 150g of MHRB for processing at once. The beaker and stirrer work fine atm, the stirrer won't fit much larger of a container on it anyways, and doing 50x3 isn't bad. I'd love to do 150x3 though lol.

3. As you state in a later post, I'm going for multiple aggitation and settle cycles, at least 4. Also my slow cooker holds two beakers as a hot bath, so 5 minutes of a vortex, then 10 minutes sitting in a heat bath works well while I do 5 minutes of stirring for each of the other two beakers.

4. Maybe it's because I'm using too small of a jar, or maybe it's the VM&P, but as far as "pouring off" the solvent, in almost all my freeze precipitations, the DMT doesn't just stick to the bottom or sides and is often free floating around as particles. I can't see a way I'd pour or pull any off without losing DMT in the process.

5. I like the idea of full spectrum results. I may pick up some Toluene, or Xylene, as that seems to be the closest I'll find in a store near me. I've already planned to grab Heptane to use for re-x in the future. I read your post on back salting, tbh it was a little dense and I'm tired so I'm gonna have to read it a few more times to understand everything in it, but it sounds like it makes a lot of sense.

no prob Macrohard



For 100g MHRB is needed 2L bottle (1,5L water + MHRB + NaOH + non-polar), 5L bottle can do 300g. I have all sizes from 100ml up to 5L.



I would say it may be due to low saturation. My process is different, I am using very saturated heptane and slow crystallization (room=>fridge=>freezer). I am never using the non-polar from pulls for freeze-precipitation, but rather continue with mini-A/B and heptane re-x. Because the dmt is dissolved while the heptane is hot and then it cools down to room temp leaving impurities behind, it is much more saturated than if the dmt is dissolved in room temp heptane.

What you can do if you have to use the filter is washing it afterwards with acetone or hot naptha and evaporating or recrystallizing or using this naptha for next pull. You won't lose anything.



If you wanted to go this way, do not hesitate to ask. Basic info here

Hey @pete666 thanks for all the information again. I've been spending the last few hours reading and trying to make sure I'm ready for the changes I'm making to the process. I'm having trouble taking the concepts Im reading though and putting them into physical practice.

Hoping you can guide me a bit based on your process and what I've done so far.

So far I've:

1. Put 500mL Distilled water into a 2L reagent bottle

2. Added 100g NaOH

3. Went to add the powdered MHRB, but I didn't have a proper funnel to get it through so added about 150mL distilled water to the bark to make it into a nice paste that would slide into the reagent bottle, I have a better funnel already for next time.

4. Shook the fuck out of it and have let it sit about 22 hours so far, shaking every few hours or more whenever I remembered.

Next I'm going to be adding another 850mL of distilled water and shaking it some more before I add my NP of choice and continue pulling.

I'm going to be using Xylene for my pulls.

So it sounds like what I would like to do is use the HCl Salting/Titration you recommended to get the goods from the Xylene into an water aqueous form or whatever, then you are basifying the water again(by adding a proportioned amount of NaOH?) before adding hot heptane for hot heptane pulls. Then you take that hot heptane and move it from the room to a fridge then freezer over a period of time then letting sit over night before pouring off the heptane and scraping off all the crystals once they are dry and then I'll have DMT. This is Freebase DMT correct?

Does that sound right in theory? If so,

when it comes to the HCL Salting/Titration, I took that mescaline calculator that was there and am trying to adapt it for DMT. Any tips on this? Should I just put 1G for estimated freebase weight in material if I'm processing 100g bark? I'm assuming the hCl information will be on the bottle of the HCl I get tomorrow. I put in the DMT Molar weight. Am I doing this right? Lol. Honestly the calculator is confusing me.

But basically I put distilled water in with they xylene, then add HCl a little bit at a time and warming to 60-80C and keep checking the pH of the water layer until it goes neutral/acidic, then I can take the water layer and perform a mini-A/B with hot heptane on it from there? Is the calculator to make those iterations less so and make things more precise in the future? Still confused on that part.

How is this mixture of Xylene/Water/HCl for emulsion? Like, your process sounds like you worked really hard on making sure no NP was in your water samples. Could I reasonably mix everything well in a flask or beaker and warm it in there, then transfer to a separatory funnel for collection of some of the water layer to test the pH before returning it all to the same vessel and adding more acid and heating again if needed then back to the separatory funnel? then once the water goes basic/acidic, move it to another vessel to await hot heptane pulls. I haven't ever had issues with emulsion on my previous basic STB extractions and tbh am not even totally sure what it would look like or mean in this specific situation. Feels like I'm being told to watch out for something but have no clue what that something is.

Can I keep that water/alkaloid layer sealed for a few days if needed and keep adding more titrated pulls to it before doing a heptane pull on all of it, or is it better to just go ahead and do a heptane pull and not wait?

Thanks so much everyone for your ongoing help!

Hey @pete666 I have a question about how you measured your titration.

Is there a reason you went through the hassle of getting water samples and testing their ph every time instead of using an indicator like this one: 1% Indicator Solution

I asked one of my chemist friends I’ve known forever about it finally as well and they suggested using an indicator like this especially since a heptane wash afterwards will likely remove any trace of the indicator. Would prevent having to constantly Pipette small amounts out and make things overall simpler right?