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DMT fumarate conversion comparison (pics) Options
 
obliguhl
#41 Posted : 3/29/2011 10:57:13 AM

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I second this question. I should be much more convinient to freeze it overnight, then thaw it...
Would the quick preciptation yield a less clean product ?

 

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endlessness
#42 Posted : 3/29/2011 11:03:27 AM

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yes quick precipitation yields a less clean product, check in the wiki where I added this tek, Ice House's 10 minutes conversion is also added there, and it yields some kind of tan resin and not white crystals.

And lorentz, after precipitation occurs, why would you evap the water? First of all, water takes a lot of energy/time to evaporate, but even if you do, what you'll get is basically all the sodium carbonate and sodium fumarate from the neutralization (the dmt should have precipitated already). You could, if you want, evap the water and then pull with dry acetone or IPA and evap to see if you can get any more alkaloids. I have a feeling if so, quantity will be very small, if any, if you did everything right before, but of course it would be wonderful if someone tested and let us know Pleased
 
obliguhl
#43 Posted : 3/29/2011 11:14:23 AM

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Ah, now i feel dumb, could have figured that out myself as I've actually read Ice Houses tek.. Sorry Embarrased
 
plumsmooth
#44 Posted : 8/6/2011 4:45:56 AM

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Couple of things please...

Sodium Carbonate solubility in Water is apparently 216 grams/liter.

That means that when trying to saturate 100ml, 21 grams can simply be used.

Also swim was in a rush and ended up dumping close to 30ml saturated solution for 1.14 grams spice dissolved in 100ml water.

Does this seem like overkill on the basfication?

Can someone tell me a way to figure out formula for exacting the amount of Na2CO3 saturated solution to add, as to not have more than necessary sticking to crystals?

It has to do with PKA right?

At a certain PH all fumarate will transform to Freebase right?

SO with a PH meter shouldn't one be able to figure out the exact amount saturated solution to add.

Last thing: what's the best way to clean the spice after this conversion?
Thanks again....





 
endlessness
#45 Posted : 8/6/2011 1:41:29 PM

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If you dump it slowly as well as if it cools slowly, cleaner crystals form.

In any case, you can easily measure by eye, add a bit till it doesnt cloud anymore. Since that quantity is not much compared with the amount of total solution, you shouldnt really have problem with sodium carb contamination, that small amount should stay dissolved in water even in fridge temperatures. In any case once you retrieve the crystals, if you do a dilute sodium carb solution wash, it should dissolve more of the sodium carb and not dissolve the dmt, so thats a way to clean it
 
plumsmooth
#46 Posted : 8/6/2011 5:37:49 PM

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I was wondering how important the refrigerator cooling part is to this water re-x formula?

I also realized that the solubility of Sodium Carbonate is lessened by about 2/3 when reaching 38 degrees or so.

So what was 21 G per 100 ml is now about 7.

Well, I guess if not over based, that should still allow plenty of storage room in the water for the excess sodium carbonate.

However, for those that might approach this using warm water initially to saturate solution.

There could end up a bit more that necessary sodium carbonate in solution.

I'm really wondering (and I realize that the ceasing of clouding is a fine marker) if there is a specific PH at which freebase spice will fully precipitate out of solution?

This would just minimize any residue.

Also can someone recommend (and maybe it is truly un-necessary) a final clean up option for the water re-x?

IPA with no water will work? And one would simply dissolve and decant through a fine filter than evaporate.

Thanks...

 
endlessness
#47 Posted : 8/6/2011 5:42:30 PM

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Download the freebase percentage calculator:

Now using pKa, you can see at a given pH how much percent of an alkaloid is in salt form or freebase Smile. DMT's pka is 8.68.

as for cleaning, IPA would dissolve dmt freebase as well as most impurities except for salts like sodium carbonate and sodium fumarate from conversion (if its dry IPA/acetone). A light sodium carb water wash would dissolve polar impurities (like sodium carbonate and sodium fumarate) and not dissolve dmt.
 
plumsmooth
#48 Posted : 8/8/2011 4:57:18 AM

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Hey when you say light, do you have any idea how little sodium carbonate can be added to H2O2 to make a solution that will not undermine the crystals.

For example if I use just enough to say raise the ph to 8.68, for lack of a better number, would that suffice as a non threatening rinse.

Thank again.

P.S. I am guessing applying the rinse in a buchner funnel with suction would be the best way to clear the crystals of any residue.

One last thing though,

Can straight water be applied without much consequence for the rinse?

I remember reading such.


 
plumsmooth
#49 Posted : 8/15/2011 12:53:58 PM

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So my friends results are in.
1.14 G Fumarates became .456 FB.
There was no disappointment.
Actually the bark didn't give a whole lot any way and it was a bit older.

The remaining water was rather yellowish and smelled pretty strongly of Dmitrius.

The peculiar thing was that with the initial excitement of looking at the lovely light -- slightly tan -- flakes on the 101 filter,

he quickly threw it into the dehydrator at only about 115-120.

I guess the initial blast of heat started to melt the lot with the exception of a few light crystals that remained on the outskirts of the plate.

Anyway dehydrator was turned down to 95 and things stabilized.
However, now, they were a darker orange-ish yellow color.
And they didn't seem to want to dry very fast.
Left them out over night and they scraped up easily; but they retained their darker color overall...

But one mystery remains: Is Dmitrius a CHAMELEON of sorts.
My friend wants his nice light white/tan fluffy flakes back.

He feels stupid that he rushed the drying process.

Why in the world have they changed color?Confused

Thanks for the feedback...


 
endlessness
#50 Posted : 8/15/2011 10:27:27 PM

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Straight water could in theory be used for the rinse since dmt shouldnt be soluble in water (unless its for some weird reason an acidic water). But just to make sure, you could do a dilute sodium carbonate solution instead, which would make sure no dmt will dissolve in it, and it will still clean well of other polar impurities (such as excess sodium carb, sodium fumarate, etc).


As for the darker color due to warm dehydration, could be a superficial oxidation? In any case it shouldnt be anything to worry about. Smoalk it up Very happy
 
plumsmooth
#51 Posted : 8/15/2011 10:36:39 PM

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Quote:
As for the darker color due to warm dehydration, could be a superficial oxidation? In any case it shouldnt be anything to worry about. Smoalk it up


Hey thanks, you're probably right.
I guess that means just a bit of oxide creeping in maybe.
Next time slow cure for those babies.

Anyway, thanks for the tech...

Between Lime, Limonene, Fumaric Acid, and the final Na2Co3 transformation,

Swim is in a personal position he never thought he'd be in 10 years ago slowly watching this developing consciousness evolve.

And even though the smoke route in not his preference:
He will have to make an exception at this point to honor and pay homage to the spirit molecule!

He may try to integrate a little fumarate/harmala pre reality check warm up to soften the sometimes harsh effect of reality in one's face Fast...

Thanks agin for sharing the wisdom!!!


 
plumsmooth
#52 Posted : 8/17/2011 2:29:43 PM

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Quite simply amazing.
Not even a trace of foreign residue.
Much smoother than the just-drying gooey acetate convertion.
Matter of fact I don't think one could call this smoking, if done properly.
Even taste good!
My friend's early days of melted orange spice on raspberry leaf and then smoked in pipe seem ghetto comparatively.
Not to mention the effect on the Lungs...
Kind of changes my whole perception of this form of administration; and is leaving me thinking I may have to incorporate this into the healings.

Still think with that nice lotus lighter VG sells with their GVG a break though may be harder to generate.
So my friend is looking at torch lighters and just read the post about the ARC.

However I see that there are many to choose from, the main criterion being a pistol or horizontal angle to save one from overly inverting their wrist.
I feel pretty spoiled with that last commentEmbarrased

Anyway thanks again...

BTW, I decided one simple way to extra minimize any residue (which already seems relatively non-existent)
is to allow the crystals in water to warm up to room temperature in solution for a day before filtering.

Cold water -- fridge temp -- holds about 3X less Na2CO3.
So I think that move makes for smoother filtering/decanting...



 
endlessness
#53 Posted : 8/17/2011 3:35:25 PM

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Awesome!

Thanks a lot for sharing your experience. I agree that water crystallized spice is of a totally different order of smoothness as compared with other methods. I wouldnt have it any other way now Smile

Cool idea about letting the solution warm up to room temperature, it makes sense and spice should anyways not dissolve back into solution so you're onto something there!

As for the lighter, I have the ARC, which is really great (and not that it really matters but it looks really epic together with the GVG, adds to the whole 'ritual'Pleased. It also has a very long warranty, dont remember how much maybe it was 5 years or something?

In any case Im sure other torch lighters with bent shape will work just fine. Before the ARC I had some cheap china-made 2-bucks torch lighters but they were extremely unreliable and broke very quickly, so make sure you get something with warranty and good reviews Smile
 
plumsmooth
#54 Posted : 8/17/2011 8:30:58 PM

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I guess I'll see if I can find one for U.S. shipping then.

Part of it is tendency to be one of these fellows who doesn't like to try to hit again after first draw.
Therefore I think torch needed to get deeper and belongs with the protocol.

Part of it is unfortunately the fear that hasn't been conquered yet.

I don't know why it is there though (of course this belongs in a different section of forum);

The warmth I felt in my heart chakra upon initiation was very loving.
And once one is in trance the mental stuff lingering is just chitta.
I'm sure properly there and the chitta will dissolve entirely.

It is not an easy path because it takes a lot of courage.
The vaporizing is so instant and one knows -- or doesn't know what's coming.
Whereas with ingestion, one has time to acclimate.

Vaporizing is like jumping off a cliff.
Maybe the two styles can converge with the use of Harmalas, and or mild pharma foundation.

Thanks aging for sharing; this place represents the hope for communion.
And you folks are my teachers...
Sharing for the love of sharing the light...

P.S. I don't think there is anything close to re-dissolving with room temp carbonate solution.
However crystals may have softened because cold they seemed to "tink" sound the glass when bouncing around.

BTW, half pint mason jar perfect for 1 gram fumarate conversion.
Instead of draining of the floaters and leaving behind the stuck-on-bottom spice to drain upside down.
Butter knife was gently applied and bottom came up in a round sheet like layer that broke in 2.
Then larger pieces were broken up just slightly.
Jar agitated, then pour in buchner = perfect vacuum drain -- to dry.
Dehydrator mistake, heat may equal oxidation turning light colored spice darker.
No problem -- smoalk it up.
In my case, the perfectionist is just a game to prolong facing the inevitable.
An attempt by fear to disguise itself through my ego -- in case you haven't figured that outRolling eyes
Silly me, personalized Zen paddle time...






 
Luuk
#55 Posted : 6/6/2013 6:51:12 PM
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I have recently recrystallized all my spice using the slow water crystallization method. It is totally awesome, so much smoother! It smells a lot less than naphtha-crystallized DMT too.

It took me some time to master, so I'll add my experiences here. These are in part just a recollection of things discovered by other people in this thread, but also a tiny experiment.

- I saturate some water with sodium carbonate, put this in the fridge to precip sodium carbonate that would otherwise precip later, then filter and use this solution.
- I then add this to my dissolved fumarates. When done slowly the impurities all stick to the bottom! If you decant the solution into another container the rest that will precip is very white! Of course the impurities that stick to the bottom still have quite a bit of DMT in them, but you can separate light yellow DMT into yellow and white DMTSmile . I've done this numerous times, and most of the time this works perfectly.
An example, I used some dark DMT and decanted, leaving me with dark freebase in one container and this in the other:



- Definitely wait the full 5 days or longer, water crystallization takes it's sweet time. Freezing and thawing your solution will give some more crystals. Even after waiting a week and freeze-thawing there was still DMT left in the carbonate solution, a small but significant amount (5-10%). I've had this every time. Do NOT throw your water away. Instead pull again with naphtha to retrieve the last bit of DMT.
- The idea of letting your jar warm to room temperature is a good one, I do this every time it ensures no sodium carbonate crystals are stuck between your DMT.
- However, without vacuum filtration, there is a lot of sodium carbonate contamination if you don't wash your crystals after collecting them. This is no problem, only if you want purity. I found contrasting information on how to further clean this contamination off my crystals.

Water washed are advised, which left me wondering because DMT has a pKa of 8,68, so if tap water was used part of the DMT would be in salt form and thus dissolve, I thought. Can someone please elaborate if this thought is correct?
An ammonia wash apparently would dissolve part of my DMT. Again, what is the proposed mechanism behind this? When using a pH 11 solution of ammonia, how can DMT dissolve? Ammonia would be the perfect base because it evaporates away.
A sodium carbonate wash would leave me with contamination because a significant amount of sodium carbonate is needed to get the washing water basic enough.
A sodium hydroxide wash is never mentioned because it is a strong base and people prefer not to have this in their product, even though a minute quantity would be sufficient to get the water basic enough.
This was all very unclear to me, and since I love water crystallized DMT dissolving the product in IPA/acetone and filtering out the carbonate contamination was not an option.
I prepared 4 containers with 15 ml of solution in them: 1 with a pH 11 solution of sodium carbonate, 1 with a pH 11 solution of ammonia, 1 with a pH 11 solution of sodium hydroxide, and 1 with 15 ml tap water (which is pH 7,8 here). PH 11 was arbitrarily chosen because virtually all DMT is in freebase form then.
In every one of these containers I put 500 mg of fairly pure, water crystallized DMT with sodium carbonate contamination. The pH of the tap water container rose to 10,4 upon adding the DMT. The containers were left for an hour in which they were occasionally stirred, then the DMT was filtered out and weighed.



The results: DMT from all containers weighed in at about 440 mg, only a few mg difference. It seems the ammonia did not have a detrimental effect on the yield.

One question remains: the excess sodium carbonate raised the pH of the tap water container to 10,4. If pure DMT is put in tap water, won't part of it dissolve?

Before that question is answered I'll stay on the safe side and use pH11 ammonia solution to wash my crystalsSmile.
 
dooby
#56 Posted : 12/11/2013 12:52:20 AM

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I haven't read the entire thread yet but I will later as there is much education and inspiration to be found here Pleased Thanks, you guys...

My experience so far...

Salting toluene with citric acid - works
- doesn't require saturated solution
- doesn't require filtering
- doesn't require evaporation
Basifying the citric acid soln. with NaOH soln. - works
- creates food-safe byproduct sodium citrate
- sodium citrate shouldn't precip from soln.

After approx. 32 hours the solution was filtered, crystals are drying for weighing purposes.
The remaining solution was combined with a fresh batch of solution and is now sitting in the fridge again.

The beauty so far: no need to dehydrate any fluids, no need to evaporate anything, crystals are looking very nice and white...

One thing I am wondering about - Will a non-saturated solution yield a less-contaminated product than a saturated solution?

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dooby
#57 Posted : 12/11/2013 10:01:06 PM

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Hello again,

I've read a few more posts in this thread...

-questions concerning "stuff that floats and stuff that sinks"
-questions concerning "more stuff precipitates than could reasonably be expected"

Whether something floats or sinks: density
Whether something precipitates that shouldn't or isn't expected: solubility

Regarding solubility: in the end the solution will be cooled in a fridge - why not cool all liquids to this temperature before saturating them with anything? It seems quite logic that a solution that was saturated at room temperature can't hold the same amount of "stuff" when nearly freezing? Also, two chemicals may be perfectly soluble in water before any reaction occurs, but checking the solubility of the reactions "by-products" may be useful as well?... It should be possible to make sure nothing precipitates but the alkaloids, or am I missing the point?

Regarding density: if I understand things correctly things float if their density is lower than the density of the solution they're in - they sink if they're denser than the solution... As long as one knows the density of a compound, the solutions density could be adjusted accordingly to ones wish to make said compound sink or float?

Perhaps there is no hard data yet regarding the densities of some desirables, but I'll start calculating as soon as I acquire the knowledge to do so Pleased

density of dmt: 1099 kg/m³...to make a solution with a density of 1101 kg/m³ add 125 gr/litre of NaCl (this is not taking into account the increase (edit: or decrease!) in density caused by the other, already present reagents, so until empirical proof is obtained this is hypothetical)...

I hope this can be helpful to my fellow Nexians...

PLUR

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dooby
#58 Posted : 12/13/2013 8:55:45 PM

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Update...

I added NaCl to the solution containing my dmt in order to increase density without affecting pH...

The crystallisation process is slowed by the high ionic strength of the saline solution.
Therefore it is not possible to draw conclusions yet regarding the benefits of increasing density of the solution in precipitation of dmt - any benefits of the higher density are clearly negated by the higher ionic strength of the solution.

I now find myself looking for ways to lower the ionic strength again, without having to pull with an nps or without adding chemicals that would affect pH too much or create unwanted by-products...

At least I learned that ionic strength is detrimental to crystal formation, probably due to inter- or intra-molecular forces Pleased

I tried google in order to improve my understanding of what's going on, but the info I found is way beyond my comprehension Pleased
My avatar was taken from google images and is actually a work of art by NEIL GIBSON, credit where credit is due!


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