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SWIM has crystals!!......now what? *Pics added* Options
 
Methtical
#1 Posted : 9/23/2009 12:36:50 PM

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Salutations!

SWIM followed the procedure as outline in the pictoral PDF as supplied by Spice-T recently.

Basically, SWIM used 100g MHRB in 1.5L of dH20 supplemented with 100g NaOH.
SWIM shook the crap out of this for 10 minutes and left in a sink filled with hot tap water for 1 hour, shaking again every 15 minutes.
At this point, SWIM added 100mls naptha (in the form of White Spirits, heavy desulphorized) and gently rolled around with the occasionally "more lively" shake, but not as vigourous as with the MHRB/NaOH/H20 mix.
SWIM left this in the sink filled with hot water for 1 hour before pulling off the top layer and placing it into a collection vessel.
Another 100mls of naptha was added, again left for 45mins, and the top layer pulled.
The third addition of naptha was left to seperate overnight and then pulled.
A fourth pull was also made (100mls naptha was added with each pull).

SWIM then took care to pour the contents of his collections jar into another whilst attempting to remove as much visible MHRB remnants which had managed to be transferred despite SWIMS best efforts.

SWIM then performed a carbonate wash. He used anhydrous sodium carbonate which reached a pH of 11.5. SWIM poured roughly 50-100mls of carbonate solution into the collection vessel and shook the crap out of it. SWIM saw a visible crystalline layer form at the bottom, and seperated the top layer which was retained.

A second carbonate wash was then performed with similar results, although less crystalline solution was formed at the bottom. Finally, SWIM added some tap water and shoook the crap out of it. A milky kind of layer was formed at the bottom, and the top layer was seperated off again and retained.

SWIM then nuked some Epsom Salts in a microwave for 5 minutes and added these to the collection jar. SWIM then filtered these through Whatman filters, leaving only flow-through and no epsom salts.

SWIM placed his collection vessel in the fridge for ~3 hours before placing into a -20 oC freezer overnight.

This morning SWIM came to inspect the fruit of his labours, expecting to be disappointed seems as though it was SWIMS first attempt.

Lo and behold, SWIM saw crystals, and was pleased!

Some crystals on the sides, but the majority seemed to for a decent layer at the bottom of the jar. SWIM tilted the jar to see if the crystals were firmly set, which indeed they were.

SWIM then replaced the jar back into the freezer to be attended to later.

SWIM therefore is wondering whether he has the right idea of what to do next.

SWIM believes he should pour out the naptha through a filter, then, whilst keeping the jar inverted, replace the cap and place the jar back into the freezer to allow the residual naptha to pour down to the bottom without stealing any precious spice crystals. After several hours, SWIM intends to remove the jar and discard the remaining naptha solution. SWIM then believes he is to scrape out the crystals, either onto a pyrex dish or filter paper, and then leave to dry throughly. Is SWIM correct in these assumptions?

SWIM feels a recrystallisation would be favourable, as SWIMS body is a temple an all....., however, SWIM will ask for clarification on this step later.

SWIM should also add at this point that pictures will be provided later.

One final thing is that, even at this stage, SWIM would like to express his appreciation for the DMT Nexus forum members for their selflessness and patience when educating noobs like SWIM. Many questions have been answered in previous posts, which SWIM would have made himself had the members of the forum not been so gracious as to answer them for other members previously.

Methtical.
 

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SuperRad
#2 Posted : 9/23/2009 8:43:02 PM
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Seeing as you've asked the question for me, I want to know what this forum's response is to this idea:

Once one has all their nice solid crystals stuck to the crystalization jar, and the naphtha more or less decanted/evaporated, wouldn't it be a good idea to simply dissolve the dmt into acetone and then evaporate that on a plate? I figure this would be a lot more effective and time/effort efficient than trying to scrape a jar...
 
transitory
#3 Posted : 9/24/2009 10:33:32 AM

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Hi Methtical

Quote:
SWIM believes he should pour out the naptha through a filter, then, whilst keeping the jar inverted, replace the cap and place the jar back into the freezer to allow the residual naptha to pour down to the bottom without stealing any precious spice crystals. After several hours, SWIM intends to remove the jar and discard the remaining naptha solution. SWIM then believes he is to scrape out the crystals, either onto a pyrex dish or filter paper, and then leave to dry throughly. Is SWIM correct in these assumptions?


Congratulations on your friend's successful extraction!- the above sounds spot on mate- he shouldn't have any problems there.


SuperRad -
Quote:
wouldn't it be a good idea to simply dissolve the dmt into acetone and then evaporate that on a plate?


I don't see a reason why this couldn't work- it would just add another (unnecessary?) step to the procedure. I have in the past swilled my empty collection jars with warm naphtha to remove any residual DMT then added to the next pull. But I've not had too much difficulty scraping perhaps 98% of product.


"Give enough that it feels good but not so much it hurts"
Life is not a task. There is absolutely nothing to attain except the realisation that there is absolutely nothing to attain.
What is sought remains hidden from the seeker by already being everything.

(Tony Parsons)
 
Methtical
#4 Posted : 9/24/2009 11:18:50 AM

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Thanks!

SWIM inverted his jar and left in the freezer until he is able to attend to it tonight. Once SWIM has scaped out his crystals he will provide pictures and ask for advice on what to do next.

Methtical
 
Methtical
#5 Posted : 9/24/2009 6:24:23 PM

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OK, so SWIM opened the jar and poured the residual naptha off into a seperate container - a fair few crystals were already present with this, SWIM was able to rescue the majority though.

The rest was scraped out and laid on a glass plate. There appeared to be variation in the consistency of the crystals - some were fluffy but it was clear that they need to be tried out further, others were in a kind of mush - again SWIM is hoping that once the naptha evaporates these will be fine too.

However, as can be seen in the picture, the bottom of the jar had much of these orange/yellow paste in which many crystals were embedded. SWIM did his best to keep these seperate from the nice looking crystals, as he is not sure what this stuff is and whether it is of any use (could someone clarify this for SWIM?).

SWIM intends to leave this out in the open for a couple of days to see what transpires, then SWIM will decide on whether to perform a recrystallisation, but does not know if it would be necessary for the nicer looking crystals?

SWIM thought about hooking up a fan to assist in this, but has read that this can lead to all DMT converting to the not-as-good N-Oxide form, so figures that perhaps leaving it to air dry might be the best solution.

Any opinons/insights would be greatly appreciated.

Methtical
Methtical attached the following image(s):
IMG_0225.JPG (1,472kb) downloaded 206 time(s).
IMG_0226.JPG (1,284kb) downloaded 206 time(s).
 
preschooler
#6 Posted : 9/24/2009 7:10:52 PM

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a fan can be used for long periods of time ...with no problems...i have no idea where you got that bad info...

looks like some decent stuff...i would just wait till its 100% dry then toss into a bubbler with some sort of leaf and smoke away.
 
endlessness
#7 Posted : 9/24/2009 7:17:02 PM

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its normal to have a certain variation in qualities, also with SWIM the straight pulls before re-x usually have different qualities, the bottom of the container has more yellowish stuff and the sides have whiter crystals

Just keep the white separate which should be fine for use, and put together the yellower mush and recrystalize it Smile
 
romiir
#8 Posted : 9/24/2009 10:57:45 PM
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SuperRad wrote:
wouldn't it be a good idea to simply dissolve the dmt into acetone and then evaporate that on a plate? I figure this would be a lot more effective and time/effort efficient than trying to scrape a jar...


YES! It is a wonderful easy way to extract the jars, however, SWIM recommends ethanol, since its cheaper, easy to make at home, etc.. Acetone is expensive and will not dissolve fumerate salts. Ethanol will dissolve alkaloids in any form and evaporates nearly as quick.
 
soulfood
#9 Posted : 9/24/2009 11:15:05 PM

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SuperRad wrote:
Seeing as you've asked the question for me, I want to know what this forum's response is to this idea:

Once one has all their nice solid crystals stuck to the crystalization jar, and the naphtha more or less decanted/evaporated, wouldn't it be a good idea to simply dissolve the dmt into acetone and then evaporate that on a plate? I figure this would be a lot more effective and time/effort efficient than trying to scrape a jar...


When I'm doing large extractions, I always do this. I just collect the dmt in acetone until the bark is exhausted, then I add a little naphtha to the mix and let it evap. The naphtha slows down the evaporation so the crystals don't turn gooey.
 
Methtical
#10 Posted : 9/24/2009 11:31:35 PM

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romiir wrote:


YES! It is a wonderful easy way to extract the jars, however, SWIM recommends ethanol, since its cheaper, easy to make at home, etc.. Acetone is expensive and will not dissolve fumerate salts. Ethanol will dissolve alkaloids in any form and evaporates nearly as quick.


Wouldn't it be necessary to use 100% ethanol though to avoid the minute water percentage dissolving the DMT? If so it's a shame SWIM didn't know this before since he has access to pure ethanol......I guess theres always next time!

SWIM took the yellow goo and used a minimal amount of warm naptha to re-dissolve into solution. There was a small brownish residue that didnt seem to want to re-dissolve - SWIM figured that this was probably crud that is not desired and so left it as it was.

SWIM then placed a tissue over the top of his shot glass and punched lots of holes in the top to still allow the naptha to evaporate. SWIM figured he would let it sit for a few days at room temperature to evaporate slowly and hopefully produce some large clear crystals - or should SWIM have headed straight for the freezer again?

Methtical
 
romiir
#11 Posted : 9/24/2009 11:40:14 PM
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Methtical wrote:
romiir wrote:


YES! It is a wonderful easy way to extract the jars, however, SWIM recommends ethanol, since its cheaper, easy to make at home, etc.. Acetone is expensive and will not dissolve fumerate salts. Ethanol will dissolve alkaloids in any form and evaporates nearly as quick.


Wouldn't it be necessary to use 100% ethanol though to avoid the minute water percentage dissolving the DMT? If so it's a shame SWIM didn't know this before since he has access to pure ethanol......I guess theres always next time!

SWIM took the yellow goo and used a minimal amount of warm naptha to re-dissolve into solution. There was a small brownish residue that didnt seem to want to re-dissolve - SWIM figured that this was probably crud that is not desired and so left it as it was.

SWIM then placed a tissue over the top of his shot glass and punched lots of holes in the top to still allow the naptha to evaporate. SWIM figured he would let it sit for a few days at room temperature to evaporate slowly and hopefully produce some large clear crystals - or should SWIM have headed straight for the freezer again?

Methtical


Ethanol azeotropes at about 95%, theres no such thing as 100%. DMT and DMT fumerate are water and ethanol soluble so it doesn't matter, it just effects evap time if you have more water to get rid of.

The brownish goo is probably some of SWIMs basified solution which was emulsified in with SWIMs napatha, it is very good to get that out of SWIMs spice. Smile

At this point SWIM would recommend evap'ing it, since there is no need to freeze it again and have additional losses.

Ethanol evaporates more quickly than napatha with less smell in SWIMs experience. (Breathing ethanol wont hurt you, breathing napatha is really bad.)

Best of luck in your quest to enlightenment!
 
endlessness
#12 Posted : 9/24/2009 11:51:10 PM

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romiir wrote:
SuperRad wrote:
wouldn't it be a good idea to simply dissolve the dmt into acetone and then evaporate that on a plate? I figure this would be a lot more effective and time/effort efficient than trying to scrape a jar...


YES! It is a wonderful easy way to extract the jars, however, SWIM recommends ethanol, since its cheaper, easy to make at home, etc.. Acetone is expensive and will not dissolve fumerate salts. Ethanol will dissolve alkaloids in any form and evaporates nearly as quick.


so you got me curious.. how to make ethanol? Is it possible without spending too much money? I would love to have some still but always been put off by the prices of stills and didnt find any practical 'do-it-yourself' plan
 
Methtical
#13 Posted : 9/25/2009 12:01:23 AM

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romiir wrote:



Ethanol azeotropes at about 95%, theres no such thing as 100%. DMT and DMT fumerate are water and ethanol soluble so it doesn't matter, it just effects evap time if you have more water to get rid of.


Ahhh SWIM was thinking that water was a no no as soon as all pulls had been made from MHRB/NaOH/H20 mix, but I guess this is to make sure the DMT resides within the naptha and is not lost in the water. Thanks for clearing that up!

Quote:

The brownish goo is probably some of SWIMs basified solution which was emulsified in with SWIMs napatha, it is very good to get that out of SWIMs spice. Smile

At this point SWIM would recommend evap'ing it, since there is no need to freeze it again and have additional losses.


Cool, glad to know SWIM is thinking in the right direction.


Thanks again!

Methtical
 
romiir
#14 Posted : 9/25/2009 12:01:32 AM
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endlessness wrote:
so you got me curious.. how to make ethanol? Is it possible without spending too much money? I would love to have some still but always been put off by the prices of stills and didnt find any practical 'do-it-yourself' plan


Well its a pretty straightforward process, get ahold of some distillers yeast, a 25 lb bag of sugar from your local market and some jugs/carboys find out the specifics for SWIM's yeast (most are labeled, and there is an optimal amount of sugar), probably 18-21% alcohol in 48 hours, (24 hours with some of the awesome scary superyeast).

Then take that, and heat it till it starts boiling, recollect (condense) the vapor into another container and you will have nearly 95% ethanol. Just make sure your temp never hits 100C, alcohol evap's at 90C. If you go over on temp you will have more water in your alcohol, however it will still be very strong stuff. Wink

There are many home distillation kits on ebay for $60-$90 ranging from 1 gallon to 4 gallon if you are not inclined to make your own.

It is very useful since you can distill anything in it, even water, Smile

Of course swim must be careful that he has a license to distill ethanol... Rolling eyes
 
Darkbb
#15 Posted : 9/25/2009 12:36:07 AM
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Those are some sexy pictures. First in a while. SWIMS next extract w/ have pictures of the product ( SWIM said that last time too but the product wasn't of significant quality to post)

Good luck

Peace and Solid
 
SuperRad
#16 Posted : 9/27/2009 5:55:32 PM
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soulfood wrote:
SuperRad wrote:
Seeing as you've asked the question for me, I want to know what this forum's response is to this idea:

Once one has all their nice solid crystals stuck to the crystalization jar, and the naphtha more or less decanted/evaporated, wouldn't it be a good idea to simply dissolve the dmt into acetone and then evaporate that on a plate? I figure this would be a lot more effective and time/effort efficient than trying to scrape a jar...


When I'm doing large extractions, I always do this. I just collect the dmt in acetone until the bark is exhausted, then I add a little naphtha to the mix and let it evap. The naphtha slows down the evaporation so the crystals don't turn gooey.


Could you elaborate on adding naphtha to the acetone? I've definitely had acetone give me gooey results, I had no idea that was because it was evaporating too fast! Do you just eyeball a splash of naphtha? How much acetone do you have at this point?

Here's an extraction experiment I have planned:

STB with Toluene. FASA. Wash the fumarates with toluene and acetone. Dissolve with water. Defat once more with Toluene if the water is not crystal clear. Then add acetone to the water and add NaOH and rock salt until the DMT freebases and the acetone and water separate, the acetone should now have all the DMT freebase, ready to be evapped on a plate!

What do you think?
 
Methtical
#17 Posted : 9/28/2009 2:45:55 PM

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Ok SWIM figured he would update on his situation.

The crystals no longer gave off an odour of solvent, and they looked more crystalline and sparkly, SWIM figured this was the sign of a finished product. SWIM had used White Spirit as his Naptha source, and it only took 1-2 days to evaporate completely, which was pleasing as SWIM was expecting it too take substantially longer.

So SWIM collected all crystals together in a 5ml tube. He blanked his scale against an empty one and compared. The final product was 0.6g, which SWIM realises is not THE best yield from 100g of MHRB, however, since it was SWIMS first attempt, he is still quite pleased with himself, and of course along the way figured out a few tweeks here and there that will be implemented into the next attempt that should hopefully improve this final product. SWIM is just pleased he produced nice, clean looking crystals, since he has read many a thread where people are having problems and would hate to be in that situation.

In addition, SWIM took all the yellow crap featured in the above pics and began a recrystallisation, however he is evaporating the naptha and this is taking a long time, nonetheless, SWIM is seeing some crystal shards much akin to other pics posted in various other threads within the nexus, and they look great, however, SWIM was not able to capture these on a pic because of the roundness of the shot glass - it doesn't alow for pics that do any justice, so SWIM will post these as and when.

Methtical
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gammagore
#18 Posted : 9/28/2009 6:15:39 PM

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Now you need to fire up that pipeSmile
 
transitory
#19 Posted : 9/28/2009 7:34:39 PM

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Thanks for updating Cool

My friend also is happy once he can describe his product as 'crystalline and sparkly'. Those crystals look good and should smoke smooth.
Others here seem to have gained clean crystals with white spirit.

Bon Voyage my friend Very happy
"Give enough that it feels good but not so much it hurts"
Life is not a task. There is absolutely nothing to attain except the realisation that there is absolutely nothing to attain.
What is sought remains hidden from the seeker by already being everything.

(Tony Parsons)
 
Methtical
#20 Posted : 9/28/2009 8:14:17 PM

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transitory wrote:
Thanks for updating Cool

My friend also is happy once he can describe his product as 'crystalline and sparkly'. Those crystals look good and should smoke smooth.
Others here seem to have gained clean crystals with white spirit.

Bon Voyage my friend Very happy


Yes it seems very good for freeze-prep but god awful for evap, so SWIM is thinking that Acetone wash would be an excellent combination for the future. The beauty of white spirit is it's cost and availability.

SWIM will let you know how the journey pans out.

Methtical
 
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