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Is losing 62% product by washing normal? Options
 
blue.magic
#1 Posted : 7/24/2017 9:56:03 PM

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After carefully following Cyb's Max ION Tek, I obtained 970 mg yellowish spice from 100 g MHRB powder. That is 0.97% yield.

However, by redissolving in heptane, separating from orange goo, washing the solvent and freeze precipitation, I was left with only 230 mg.

I left some of the goo as well as leftover heptane from freeze precip. to fully evaporate to give me some 140 mg yellow-ish/orange-ish spice, that still almost 62% loss!

Is this normal?

People often report yields of 0.7-1.5% but even after several trials, I still can't get over 0.3%.

Could this be a weak MHRB? I don't know what am I doing wrong: enough lye (also tried KOH), tried different acids, salting the water, heating both solvent and the water, recycling alkaloid-containing solvent, pre-evaporating, washing every container with solvent three times etc. following almost analytical lab techniques, yet I still can't get even close to yields obtained by many with much simpler approach.

I tried A/B, STB, ATB and the result is always the same - very small amount of product.

People say it's cheaper to make DMT yourself, but for me it's several times more expensive due to such diminishing yields.
I want to keep making it myself though, because I want to know what chemicals were used and make sure it is absolutely food safe.
 

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Ulim
#2 Posted : 7/24/2017 11:41:56 PM

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Do you use the same bark only? Maybe try some different one.
And also try to smoke the part of the spice you removed and see if its active.
Also if you use KOH you have to remember that you need to use more of it because K being heavier than Na. You need to calculate the right moles. In this case multiply the NaOH used by 1.4 to get the amount of KOH to replace.

Imo you have just craptastic bark. Or you messed up the cleanup hard. Thats why you should try to smoalk what you removed.
 
blue.magic
#3 Posted : 7/25/2017 12:07:44 AM

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The orange residue is normally active, just like pure DMT (I can't tell the difference), but there is quite a lot of it compared to the white stuff (like 20% or so).

Most of the losses are in the heavy oily orange gunk that remains after redissolving in heptane (I use naphtha for pulling, then heptane for washing/re-x ... once separated, the residue refuses to dissolve even back in hot naphtha and most of it is lost because it sticks to glass). It is active but I can't and don't want to use it for vaporizing as it messes up my glass pipe and is hard to weigh. I keep it for changa though.

Okay I will try a different vendor, that's a good idea.

Maybe I will also switch to standard A/B extraction with defatting. The advantage of STB breaking down the root bark using strong base seem not being worth for all the fats being pulled (even the recrystallized product tends to stick on the vials).

The naphtha is more colored with each pull and more messy also. If I won't heat it though, I'm afraid it won't pull all the spice.
 
Ulim
#4 Posted : 7/25/2017 12:42:41 AM

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I dont heat and get good yields.
Heating means lots of goo and gunk. You are basically turning all the fat into soap.
 
blue.magic
#5 Posted : 7/25/2017 12:21:34 PM

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Thanks for the advice. I thought saponification has more to do with too high pH rather than heat.

The Tek says:

Quote:
Add minimal amount of ‘warm/hot’ NPS


So I guess just 'lukewarm' (i.e. 35-40 degrees C) would be fine. But I would keep the tea at room temperature...
 
Ulim
#6 Posted : 7/25/2017 12:57:39 PM

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Saponification happends very slowly at high ph.
"Cold" Soap needs week to fully react.
Heat that and you shorten it to a day or two.
 
endlessness
#7 Posted : 7/25/2017 1:11:13 PM

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If you dont throw anything away, nothing is lost.. For example, how much solvent you used for the re-x? Also, the orange goo that stayed behind during re-x, did you do another pull on it and freeze/evap separately? Usually there's more DMT there if you only used a small amount of warm solvent.

Also, how did you wash the solvent? pure water? water+base?
 
blue.magic
#8 Posted : 7/25/2017 5:23:01 PM

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endlessness wrote:
how much solvent you used for the re-x?


About 10 mL hot heptane, mixed thoroughly, let the orange goo settle and decanted heptane to a 250 mL sep. funnel. Then repeated this two more times hoping most of the DMT transferred to heptane.

The amount of goo was about 1.5 mL so I though not much DMT could be left there as it would have more incentive to distribute in total of 30 mL of 99% pure fresh heptane rather than stay in the goopy fatty residue.

So there was about 30 mL heptane in the funnel and I followed with water wash. The heptane layer has been poured to a Pyrex dish and the funnel has been washed two more times with fresh heptane to get any leftovers out.

endlessness wrote:
If you dont throw anything away, nothing is lost.. For example, how much solvent you used for the re-x? Also, the orange goo that stayed behind during re-x, did you do another pull on it and freeze/evap separately?


I mixed the remaining orange goo with small amount hot naphtha, mixed tohroughly and then poured on dish and completely evaporated. Significant amount of the goo stayed in the glass because it sticked to it - it didn't even dissolve in naphtha and I didn't want to use more aggressive solvents.

Maybe I could remove most of it using spatula, it was like a thick oil. But at this point I thought most DMT is in the heptane (apparently it wasn't) so I just poured few drops of the goo on dish to evaporate - the nastiest part was discarded unfortunately.

endlessness wrote:
Also, how did you wash the solvent? pure water? water+base?


10 mL water with a pinch of sodium carbonate (20 mg or so)
then 2x 10 mL distilled water (as suggested by Vovin's Tek)
 
Asher7
#9 Posted : 7/25/2017 5:28:58 PM

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Just for clarity, I've read a few times where people say to pour your solvent into your bark sludge and stir, let settle, stir, let settle, pull. Like the solvent shouldn't be in there for more than 5 minutes. Is this thorough? I thought you were supposed to let it stay in there "overnight" stirring semi-frequently so it can get good and saturated. (STB)

@Blue, I'd second the switch up bark recommendation. I've heard stories of people having "MHRB" that wasn't even mhrb, I think there's some subspecies + I hear sometimes the bark comes from the wrong part of the tree. All speculation, but the stories are out there..
 
endlessness
#10 Posted : 7/25/2017 6:23:57 PM

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My bet is that you still have dmt in that goo even after 3x10ml pulls. The stuff that wouldnt crystallize can be DMT. DMT is polymorphic and one of the appearances it has, even pure, is an oil. Also, oil/goo can be deceptively heavy.

You could try redissolving in small warm pull and freezing, or scraping/rescraping and letting dry over a couple of days to see if it hardens up...
 
blue.magic
#11 Posted : 7/25/2017 6:43:18 PM

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endlessness wrote:
My bet is that you still have dmt in that goo even after 3x10ml pulls. The stuff that wouldnt crystallize can be DMT. DMT is polymorphic and one of the appearances it has, even pure, is an oil. Also, oil/goo can be deceptively heavy.

You could try redissolving in small warm pull and freezing, or scraping/rescraping and letting dry over a couple of days to see if it hardens up...


I agree. When I evaporated the naphtha with residues I had no time left to scrape the goo, so I just left the dish on the table sitting upside down.

The next day I was suprised. It all hardened to a beautiful crystalline circles, just slightly colored!

After scraping, it became brownish, but still... I never read about the goo hardening into crystals, even after fan drying. If only I've read about it earlier...

BTW I did 50 mL naphtha pulls. 10 mL is too little to pull with a pipette or even a syringe (it always pulls mostly the brown tea even if it barely touches the surface) - I had about liter of water in a bottle with narrowing neck. To pull 10 mL - I would have to use sep. funnel but that is not possible with STB unless I wanted to make lots of mess.

10 mL is usually somehow lost in the MHRB tea. I always thought it evaporated since every time I do 50 mL pull, I end up with about 40 mL.

I also cannot stirr it as it's all in a bottle. That would require quite long and thick stirring rod maybe. Even the 5 cm magnetic stirrers I have is too small to move all the bark.

Finally just 10 mL pull makes a very thin layer in the Pyrex dish. This seem to cause fats being deposited on the bottom making the product even stickier.

The pulling is done by first shaking the bottle vigorously for about a minute. It all settles in few minutes, then I pull.
I have to wait till next day for the next pull (to use naphtha from previous pull). I also read that letting the base soup sit for days is only beneficial as more bark is broken down and it won't hurt DMT. Now I hear about the saponification issue...

...so many reasons to go back to A/B.
 
 
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