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Pure DMT Fumarate from freebase DMT Options
 
endlessness
#61 Posted : 8/21/2008 1:34:43 AM

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once again im very happy for the very intelligent dedicated psychonauts here in this forum Smile


sucks that where SWIM lives, acetone is controlled by the regulatory agencies (and so is toluene).. though pure naphtha and hexane are easy to find.. but SWIM is very interested nevertheless in what your friends find out Smile
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Infundibulum
#62 Posted : 8/21/2008 12:02:08 PM

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69ron wrote:
I didn't know freebase DMT would settle down out of the water after 1-2 days. Are you sure about that?

Man I love your ideas. The washing machine is indeed a centrifuge, especially the one I own. That sucker spins REALLY FAST. That gives me some new ideasSmile


From SWIM's observations it should take a good 2 days for the milky solution to sediment, in which case one would be able to see some crystals in the bottom plus clear crystals attached on the sides of the tube (at least in SWIM's polypropylene tubes). The ones on the side are difficult to wash, SWIM had to decant the liquid, let all the rest of water evaporate (it took another 4 days to do that completely) then retrieved the spice just by washing the tube with acetone. All the residual salt (sodium fumarate) and base (sodium hydroxide) from the aqueous solution are insoluble in acetone and sediment fast.

Now, this method assumes that:

1)one has plenty of time ahead
2)dmt fumarate is dissolved in the minimum amount of water
3)base is added dropwise (both NaOH and highly concentrated sodium carbonate can do excellent work) until solution does not become more milky.

Now, a centrifuge can speed up the sedimentation time a million-fold, basically they can do it in 5 min when you apply a x18,000g force.

BUT PLEASE PLEASE PLEASE DO NOT ANYONE GO AROUND ASKING TO BUY A CENTRIFUGE! THEY ARE VERY EXPENSIVE AND DANGEROUS TO USE! THIS IS WHY SWIM IS TRYING TO FIND A SAFE WAY FOR CENTRIFUGING BY USING A WASHING MACHINE!!!!



Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
lorax
#63 Posted : 8/21/2008 2:52:24 PM

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is this tek usable or not? up there it says not to use it. can someone please rewrite this tek and post it again? that'd be awesome! also another question: when using DMT fumarate sublingually.. whats the dose range from mild to strong?
I am the Lorax. I speak for the trees. I speak for the trees, for the trees have no tongues. And I'm asking you, sir, at the top if my lungs.. (all posts are fictional and are intended for entertainment purpose only)
 
Infundibulum
#64 Posted : 8/21/2008 3:42:11 PM

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SWIM has never tried dmt fumarate sublingually. But one may be able to snort 150mg fumarate salt (= ~100mg freebase) for a ~1 hour experience which as a matter of fact did not impress SWIM that much. Plus it's a lot of material to put up the nose!

As for the tek, SWIM has t o repeat it, take good pictures and measure times accurately. But to begin with, this method started being developed as a means of what to do further with dmt-fumarate.

Chronologically, SWIM decided to use fumaricacid saturated acetone (FASA) to salt out freebase dmt from non-polar solvent. In its philosophy, it sounds a bit like Cosci's tek.

So, the basified plant material was extracted with xylene. One may pull with repeated volumes of fresh xylene if one has a lot or re-use the same tiny amount (100ml for SWIM) again and again and again. SWIM opted for the second option because hates working with big volumes of xylene; it smells nice, but it is also alarm signal for the neighbours and whoever would like to stop you from doing what you are doing.

Anyway,

a) first xylene pull (coloured piss yellow) goes in an appropriate container.

b) FASA was added dropwise, xylene became cloudy due to the salted alkaloids. One cannot put too much FASA.

c) solutions was left overnite at room temperature allowing for the alkaloid-fumarate to sediment. Now one got them out of the xylene without the need to evaporate it!

d) Xylene was siphoned off and washed with plenty of water. This was done because this xylene had traces of acetone and fumaric acid that one does not really want. Water washed away fumaric acid and acetone, leaving back clean xylene (plus the yellowy plant oils that dissolved into it). This xylene was used for the second pull etc etc. By this approach one knows when to stop pulling since at some point there will be no alkaloids in the xylene to be salted out. it took SWIM 7 100ml xylene pulls to exhaust 240g MHRB.

e) fumarate alkaloids were washed 3 times with some acetone to remove any residual xylene and oily impurities.

f) Then they were dried in the oven at 70 Celsius until pretty hard.


And this is the point where the centrifuge can be used; one can get the fumarate salt dissolve it in water, basify and pull with fresh xylene, then evaporate it to get pure freebased alkaloids. But SWIM couldn't really be arsed. So he dissolved the salts in the minimum amount of water, basified and then stuck the solution in the centrifuge to collect them.

The philosophy of the centrifuge is as such; Something is spun at very high speed usually at the range of 5000rmp (rounds per minute) to 20,000rpm, and this generates a force (centrifugal force) which effectively makes things "heavier". So, one can generate a centrifugal force of, say x 10,000g which roughly means that an object (in our case an insoluble freebased alkaloid) will behave as 10,000 times heavier. A centrifuge just speeds up something that anyway happens (i.e. precipitation).

And it is totally unnecessary; In a SWIM's pilot experiment fumarate alkaloids were dissolved in the minimum amount of water, basified and then let it sit at room temperature. This milky solution got clear after 2 days and SWIM could observe wee shiny crystals sitting on the bottom and the sides of the tube trying to protect themselves from the hostile aqueous environment...How cute!


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
69ron
#65 Posted : 8/21/2008 6:16:43 PM

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Ronue wrote:

BUT PLEASE PLEASE PLEASE DO NOT ANYONE GO AROUND ASKING TO BUY A CENTRIFUGE! THEY ARE VERY EXPENSIVE AND DANGEROUS TO USE! THIS IS WHY SWIM IS TRYING TO FIND A SAFE WAY FOR CENTRIFUGING BY USING A WASHING MACHINE!!!!


That's no joke. Take that seriously. A centrifuge can blow up sending little shards of material flying all over everything in the room if not done properly.

Here's an image of a centrifuge that blew itself apart:
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
Psychologic
#66 Posted : 8/21/2008 11:27:38 PM
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What happens if there is some residual lye in the dmt freebase that is dissolved in the acetone? One statement I noticed as I was looking around was "Acetone may react vigorously with certain oxidizing agents such as sodium hydroxide (NaOH)." (http://www.dow.com/productsafety/finder/acetone.htm)

Would this create unwanted compounds in the solution or just cause some heat like when NaOH dissolves in water? Also, would the NaOH precipitate out of the solution with the dmt fumarate or would it remain in the acetone?

 
69ron
#67 Posted : 8/21/2008 11:32:42 PM

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Good question.

SWIM uses sodium carbonate and NOT sodium hydroxide, so it's not a problem for SWIM.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
fourthripley
#68 Posted : 8/21/2008 11:38:06 PM
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I have heard a rumour of a rumour of somebody using a bicycle to 'centifuge' cactus emulsions but that really is all I know. Think it may have been effective , no idea how it was done though...
mistakes were made
 
drainlife20
#69 Posted : 8/22/2008 12:19:39 AM

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Zip tying test tubes to the spokes would work. You could take a washing machine partially apart, and rig zip ties through those tiny holes on the sides of the wall. Let's just say one were to use a jar, I wouldn't suggest glass. I mean if you really wanted you could use a glass jar, wrap it up in a towel and duct tape it so the padding would stay. That way if it did come loose, it hopefully wouldn't break.
Thanks for reading my dream diary! I hope you found it interesting! LMBO!
 
Psychologic
#70 Posted : 8/22/2008 1:18:44 AM
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69ron wrote:
Good question.

SWIM uses sodium carbonate and NOT sodium hydroxide, so it's not a problem for SWIM.

Do you happen to know whether NaOH or Na2CO3 is soluble in acetone?

 
69ron
#71 Posted : 8/22/2008 1:21:15 AM

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Yes.

NaOH (sodium hydroxide) is soluble in acetone, alcohol, and many other solvents. Most hydroxides are soluble in many solvents. <--- WRONG. SWIM TESTED IT. NaOH (sodium hydroxide) is INSOLUBLE in dry acetone.

Na2CO3 (sodium carbonate) is insoluble in acetone, alcohol, and many other solvents. Carbonates are in general poorly soluble in most solvents. Take calcium carbonate for example, it's insoluble in everything except dilute acid in which is reacts.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
Psychologic
#72 Posted : 8/22/2008 1:37:09 AM
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69ron wrote:
NaOH (sodium hydroxide) is soluble in acetone, alcohol, and many other solvents. Most hydroxides are soluble in many solvents.

Interesting. So would this mean that any residual NaOH present in DMT freebase would be removed by converting the DMT to the fumarate salt in acetone?
 
69ron
#73 Posted : 8/22/2008 1:43:49 AM

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Yeah. That should work.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
Infundibulum
#74 Posted : 8/22/2008 9:24:06 AM

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69ron, SWIM has personally found NaOH to be completely insoluble in acetone, just like Na2CO3. But SWIM's acetone is the purest possible; it IS the case however that traces of water (even absorbed moisture from the environment which are are miscible in acetone can aid the solubility of NaOH in acetone.


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
69ron
#75 Posted : 8/22/2008 7:33:29 PM

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Yes. My mistake. SWIM tested it just now. Ronue is right.

NaOH (sodium hydroxide) is indeed insoluble in dry acetone. So the source of that information above is inaccurate. Sorry about that. SWIM should test things before he posts anything he’s heard from others.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.
 
Viracocha
#76 Posted : 8/26/2008 2:58:35 AM

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I think it was Ronue that posted this,
said 5mL/100mg for dissolving fumaric acid in acetone

However I couldn't go any less than 20mL/100mg
any ideas on why?

Anyone know the solubility of DMT base in acetone?
 
Infundibulum
#77 Posted : 8/26/2008 9:42:05 AM

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When SWIM did the solubility test he found that as 20mg / ml acetone, (or 100mg /5ml as you posted). SWIM however waited almost 1 day before determining solubility; which of course gave some time for the fumaric acid to further dissolve. But to be honest, SWIM however has been lazy on fully saturating the acetone. He has just been mixing an amount of fumaric acid with acetone, wait for the excess fumaric acid to sediment (2-3min) then acetone is ready to use.

Hope that helps!

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Viracocha
#78 Posted : 8/26/2008 2:59:32 PM

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Yeah, doesn't really answer the original question but i'm glad that you confirmed what I thought at least Wink

I was just wondering because some swim did this:
1. dissolved 500mg of fumaric acid in 100mL of acetone
2. dissolved 500mg of dmt base in 75mL acetone
3. added the fumaric acid soln to the dmt soln while stirring

they expected to see a white cloud precipitate (which was indeed seen in the past by this particular swim!) but this wasn't the case this time. No precipitate formed. The solution was allowed to evaporate a little (about 50mL) and they then noticed glass shard type crystals forming in the bowl. They're wondering why this has happened? When the evap is done the xtals will be cleaned with MEK and bp measured. Not sure whether it's dmt.f or dmt, it looks like plain dmt base in fact. Could the reaction not have actually occured somehow and all the fumaric acid is still in the acetone, with the dmt base being forced out and crystallising?
 
Infundibulum
#79 Posted : 8/26/2008 4:31:09 PM

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This is pretty weird! But first my apologies; I didn't read your last post carefully; As a matter of fact, dmt freebase is extremely soluble in acetone, but SWIM has never measured a saturation point for that. 100mg easily dissolve in 1ml acetone for SWIM though, which is very efficient. And dmt-fumarate is totally insoluble in acetone.


Which means that the crystals your SWIM sees are certainly not freebase.

They cannot be fumaric acid either, since it was already dissolved in acetone. Any excess fumaric acid from the fumaric-acid-saturated-acetone added in the freebase-containing acetone is just going to find more free space in the acetone to dissolve itself and won't precipitate out.

Could that be the case that trace amounts of water might be present in acetone, thus dissolving / or delaying the appearence of dmt fumarate ?

SWIM has also found that dmt fumarate crystals that form out of xylene pulls also look like needles.

The odds are that what you see dmt fumarate! Try washing the crystals with pure acetone or MEK, they should not dissolve. And try to taste them:

dmt-fumarate tastes very similar to its freebase, with this slight sensation of burn and the familiar (for SWIM!) disgustingness Very happy

Fumaric acid tastes a bit acidic or kind of salty but otherwise fine.


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
amor_fati
#80 Posted : 8/26/2008 8:05:22 PM

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This is absolutely SWIM's favorite thread to follow. SWIM's been itching to be able to get in on this, and now he's been so inspired by it that SWIM's going to use it to extract from my pipe-cleaning xylene. SWIM's also considering using this form of spice for storage of future extractions. Is SWIM correct to assume that it's faster, cleaner and easier to recrystallize freebase from dry dmt-fumarate? Is SWIM also correct in assuming that fumarate powder is rockier and drier than freebase powder, meaning that it's easier to transfer between containers, scales, and whatnot?
 
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