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official extraction help thread Options
 
Phantastica
#881 Posted : 6/8/2010 6:18:25 AM

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hi fellas, so my question is regarding cleaning dmt fumarate crystals following a BLAB tek precipitation. In this Wiki tek: Purification of Spice Fumarate, in step 4, it says that to clean the spice, just dissolve it in water, and discard the remaining solids at the bottom (which will be fumaric acid). But i what i don't understand is: Why would Fumaric acid solids be left behind when dissolved in water? Fumaric acid is water soluble (thus FASW can be prepared). Am i misunderstanding something?Confused
<3
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
gammagore
#882 Posted : 6/8/2010 6:11:43 PM

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cyberelf wrote:
Hey everyone

SWIM performed his first extraction following the Lazy tek with MHRB (approx 50g) and Shellite as solvent. As the solvent has taken a long time to evaporate, he decided to freeze the solvent in a glass jar (first pull, of course). After a few hours he could see a few "snow cones" forming at the bottom of the jar. He waited another 6 hours or so and the number or size of the "snow cones" didn't seem to change.

So at this point he really did'nt understand what to do next. So he scrapped the snow cones off using a knife. The snowcones were just running free in the solvent. Then he filtered (using 100% cotton tshirt) the solvent into another glass jar. The remaining "snow cones" really looked more like ice or crystals. After a few minutes THEY DISSAPPEARED! They melted or something...

What happened? Please help! What could he do to successfully extract the spice? What could those crystals be? SWIM thought the spice would only melt at high temperatures. The whole thing was done at average room temperature.

Cheers



FAQ , our friendSmile
 
skrps
#883 Posted : 7/3/2010 7:40:34 PM
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hello!

after my first 100g extraction using the lime tek went reasonably well, my 2nd one from the same batch gives me a bit of a headache.

first off, yield was only half - only thing i changed was switching from zippo fluid to primus powerfuel. i figured primus fuel is a lighter naphtha so i'd need more pulls. after 4 or 5 with the primus fuel i did a last one with zippo fuel thinking it'd would get the last bit out. well it didn't. im a bit clueless here considering the same bark yielded twice the spice 2 months earlier. i did the pulls over the course of a few days to make sure all of the dmt had freebased.

the other thing wich puzzles me more is that i seem to be creating a lot of n-oxide (i prefer the white stuff). i re-x'd all my pulls in hot naphtha, decanted the yellow goo and freezed the clean naphtha, giving me white crystals of which half turned yellow again when drying the product, expecially those on the bottom of the jar, the ones on the side stayed white. i have recrystallized that spice again after trying a small amount. again yellow goo discarded etc. it is currently in the freezer. i am not blowing any air over it while drying, it is white when i take it out then part of it melts into yellow. i thought naphtha doesnt disolve n-oxides so how come i still have some after a re-x? can almost half of my spice turn to n-oxides when drying? im going to try turning the jar upside down in the fridge after decanting the naphtha this time to see if it helps.

cheers
 
skrps
#884 Posted : 7/4/2010 1:19:31 PM
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bleh Sad

looks like i lost 3/4 of my spice in the 2nd re-x. the stuff that did crystallize is nice and white, however still very waxy. upon scraping it up it almost seamed to smear along the sides of the glass creating a thin layer of almost impossible to scrape up waxy stuff. normally the white spice falls off nicely when touching.

the decanted yellow goo is crystallizing too so i'm assuming it wasnt n-oxides in the first place. it's also becoming a lighter shade of yellow. i'll give it a few more days to dry together with the gummy yellow stuff from the 2nd re-x. if it was plant oils in there, will those evap over time making the dmt crystallize more?

i've also let some of the naphtha i used for the recrystallizations evaporate a bit more and put it back in the freezer .. doesn't even seem to cloud anymore. so where did the spice go? i'm clueless as to what went wrong, used the same technique that worked well on the same batch of mhrb. maybe its the primus powerfuel?

another odd thing i noted was that the first 2 pulls barely got anything besides oily yellow dmt (maybe 50mg in total) whereas the 3rd and 4th got most of what i had. 5th pull yielded close to nothing. i sampled both the white and yellow oily stuff. white is super smooth, vapes clean with a very nice experience. yellow is a harsh on the lungs, bizarre mindfuck trip, with weird bodyload, and a headache afterwards. visuals arent as strong and defined. also it gives me this weird thing where the whole trip speeds up to an incredibly fast pace then fade away with strange auditory sensations afterwards.

anyway i guess ill be happy with the little bit of white i got, maybe try the yellow one more time then move on to a new batch.

cheers
 
fallensaint
#885 Posted : 7/4/2010 9:27:34 PM
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Hey all, this is my FIRST POST in the forums, and I'm really excited about exploring hyperspace. SWIM did his first extract today using q21q21s a/b tek using vinegar, lime, and naphtha with 100g mhrb. SWIM popped his 4 pulls into the freezer about 3 1/2 hours ago, and he has one question. The crystals that he's seeing are fairly large clumps, and TOTALLY white, not clear at all. Is this normal??? Any responses would be greatly appreciated.
 
wade
#886 Posted : 7/4/2010 9:28:12 PM

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sounds normal to me
 
fallensaint
#887 Posted : 7/4/2010 9:37:57 PM
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Wow, thanks for the speedy response. I'm glad to hear that...extremely excited, so I'm a little nervous and jittery wondering if I did everything right. I probably just need to calm down, followed the tek just like it said, so now It's just waiting on the precip.

On a side note, I am SO GLAD to have found these forums, you guys are a really awesome bunch, and extremely helpful to those of us just starting out in our explorations. Thank you all.
 
endlessness
#888 Posted : 7/4/2010 9:39:55 PM

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hope it works out.. the step of removing the crystals after freeze precipitating is a bit troublesome for some people due to the famous 'melting crystals' issue... check the FAQ, it has some suggestion to prevent this problem
 
fallensaint
#889 Posted : 7/4/2010 9:44:17 PM
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Thank you endlessness. q21q21s tek didn't mention this, so it could have been a problem. SWIM will make sure to finish the freeze precip upside down in the freezer and hopefully that helps.
 
fallensaint
#890 Posted : 7/5/2010 2:14:49 PM
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Well, swim poured off the naphtha, then finished the precip upside down in the freezer. This morning he scraped all the crystals form one dish onto a plate, and they immediately melted away. Swim is extremely frustated and depressed at the moment.........
 
Eden
#891 Posted : 7/5/2010 2:36:37 PM

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What did they melt away to? Wait for what is left on the plate, in whatever form, to dry and then scrape it up.
 
fallensaint
#892 Posted : 7/5/2010 2:41:02 PM
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Actually, SWIM thinks he knows what went wrong. The TEK said to simply decant off the naphtha and then prop the dish up against the wall to let the rest drain off. However, SWIM kept seeing people in the forums saying to use a fan to evaporate the naphtha, so he did this with his first 3 pulls, and the crystals all melted. The 4th he turned the fan off, and the crystals are all still there. SWIMs guess is that the fan blowing room temp air warmed up the thin film of naphtha still on the crystals before it could drain off, thus dissolving the crystals. SWIM is REALLY hoping that this 4th pull will be enough for at least one good dose because he doesn't have anymore MHRB.
 
endlessness
#893 Posted : 7/5/2010 2:42:28 PM

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fallensaint wrote:
Well, swim poured off the naphtha, then finished the precip upside down in the freezer. This morning he scraped all the crystals form one dish onto a plate, and they immediately melted away. Swim is extremely frustated and depressed at the moment.........


nothing is lost if you didnt throw away, the dmt doesnt simply dissapear into thin air, its still there.

check the FAQ
 
redeadnixon
#894 Posted : 7/5/2010 3:32:10 PM

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SWIM was wondering if it would be possible to do a purification of dmt.hcl with acetone, or would he have to convert to freebase first?
It is SWIM's understanding that this shouldn't work as the salt is soluble in polar solvents (ie acetone) but thought he should just check first to see if he could save time not doing the conversion.
It's not the first time we've been in this dream.
 
arimane
#895 Posted : 7/7/2010 1:41:16 AM

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Not really... I mean, dmt hcl will leave you with a goo, since it's hygroscopic, if you just put Acetone you'll get your goo dissolved.
What you can do is dont use hcl, but fumaric acid instead, and then use one of the method to get freebase from there.



Now, I got a question too:
Does DCM pull out the full alkaloid spectrum of MHRB (JimJam)?

If so, would they freeze precipitate then, or SWIM should just leave it to evaporate (in a very open and free place, since is really toxic)?

Would all the jimjam create a jim jam fumerate, if SWIM adds FASI (or FASW) to a d-limo extraction?


thanks =)

Arimane
Bad, bad english
 
redeadnixon
#896 Posted : 7/9/2010 7:33:16 PM

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arimane wrote:
Not really... I mean, dmt hcl will leave you with a goo, since it's hygroscopic, if you just put Acetone you'll get your goo dissolved.
What you can do is dont use hcl, but fumaric acid instead, and then use one of the method to get freebase from there.


Does anyone know how SWIM would go about converting dmt.hcl to dmt.fumarate?
Would it work if he added NaOH to a solution of dmt.hcl; then pull with non-polar solvent, and finally freeze precipitate or acidify with fumaric acid solution?
It's not the first time we've been in this dream.
 
endlessness
#897 Posted : 7/9/2010 7:41:07 PM

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yep that would work... freeze precipitating that non-polar will yield you dmt freebase though, but if instead you salt it out with a fumaric acid solution, then you will get dmt fumarate
 
redeadnixon
#898 Posted : 7/9/2010 7:51:55 PM

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endlessness wrote:
yep that would work... freeze precipitating that non-polar will yield you dmt freebase though, but if instead you salt it out with a fumaric acid solution, then you will get dmt fumarate


Thanks man, much appreciated Very happy
It's not the first time we've been in this dream.
 
Phantastica
#899 Posted : 7/9/2010 10:06:09 PM

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Phantastica wrote:
hi fellas, so my question is regarding cleaning dmt fumarate crystals following a BLAB tek precipitation. In this Wiki tek: Purification of Spice Fumarate, in step 4, it says that to clean the spice, just dissolve it in water, and discard the remaining solids at the bottom (which will be fumaric acid). But i what i don't understand is: Why would Fumaric acid solids be left behind when dissolved in water? Fumaric acid is water soluble (thus FASW can be prepared). Am i misunderstanding something?Confused

bump
<3
 
endlessness
#900 Posted : 7/9/2010 10:39:18 PM

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because dmt fumarate is much more soluble in water and fumaric acid is not very soluble in water (thus why only a bit of fumaric acid is needed for FASW). Alternatively, you can clean by doing a cold IPA wash, which should dissolve some fumaric acid but none (or very little) dmt fumarate.
 
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