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DreaMTripper
#121 Posted : 3/4/2014 8:59:48 PM

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Ok thanks for the reply, good to know, so in the past Ive made a fundamental booboo and mixed up the signs of 'supersaturated' with saturated. Only supersaturated goes 'milky'...
Further reading led me to here ... for the sake of cross linking .. https://wiki.dmt-nexus.me/Noman's_tek
Quote:
Kerberos would like to add to the advices given
by Entropmancer: following Nomans tek and
remarks regarding 1.5x water needed for
powered root bark and Entropmancer advices
regarding using less naphtha per pull. SWIM
used 50g of root bark to 750ml of water and
75g of NaOH, SWIM then used .6ml of naphtha
per gram of bark (.4ml did not give enough
depth to the separation layer in the size jar
SWIM was using) 7 pulls of 30ml (first pull 20ml)
yielded the following pure white precipitation;
1)101mg 2)107mg 3)72mg 4)41mg 5)23mg 6)8mg
7)8mg and 40mg off the shot glasses used for
the freeze precipitation for a total of 400mg, all
pulls were with room temp naphtha.


So a ball park ratio for solubility of dmt in room temp naptha in basic soup could be said to be between 2 and 5mg/ml obviously other variabilities that can change this.
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Du57mi73
#122 Posted : 3/4/2014 9:24:21 PM

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Average solubility I use is around 200ml/g at room temp(6Cool, and 30-50ml/g if heated, of naptha.
"I am cursed by the blossoming knowledge of my feminine ideal and she looks suspiciously like you."

"Everybody is a genius. But if you judge a fish by its ability to climb a tree, it will live its whole life believing that it is stupid." -AE
 
DmTpsychem
#123 Posted : 5/4/2014 4:35:16 PM
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Hi, does sb have general experience with column-chromatogtraphie on DMT?
Which Retardation factor could be expected, which solutable phases have rich aspects, which stationary phase has derived as favorable?

Thanks for your help

Edit: havn´t seen the topic about Rf-data in Plant Analysis and Substance Testing...
I just searched for Retardation factor
 
intosamadhi
#124 Posted : 1/23/2015 3:51:31 PM

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I have a question relating to the solubility of dmt in 'near neutral' water and sodium carbonate washing.

I usually mix up a solution of 1 tablespoon of sodium carbonate to 1000ml of water and use this to wash my NPS. I do this in a separatory funnel and after the washing i rinse out the little bit of water that remains at the bottom of the funnel with more clean 'near neutral' water. The water is a bit on the acidic side. The reason for the rinse is to try to dilute and remove as much of the sodium carbonate solution as possible before I salt out the alks with vinegar.

Reading through this thread it seems that dmt may be somewhat soluble in 'near neutral' but acidic water. is this the case or is it so negligible as not to matter?

Also since the concentration of the washing solution is not the standard 5% is there any risk of losing some of the freebase in the wash?

ps. This was answered somewhat in another thread, but reading through this thread brought up these concerns for me again, so just looking to see if there are any more opinions.
 
endlessness
#125 Posted : 1/23/2015 3:58:07 PM

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what do you mean with ' a bit on the acidic side' ? What pH?

If its really acidic then yeah you can def lose some DMT. You should wash with slightly basic water. You could make an even more dilute solution of sodium carb, and any tiny traces left will be insignificant anyways.
 
intosamadhi
#126 Posted : 1/23/2015 4:13:02 PM

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endlessness wrote:
what do you mean with ' a bit on the acidic side' ? What pH?


Meaning that when I use my 'difficult to read' little ph papers it leans more towards the acid side (more yellow than gree).

endlessness wrote:

If its really acidic then yeah you can def lose some DMT. You should wash with slightly basic water. You could make an even more dilute solution of sodium carb, and any tiny traces left will be insignificant anyways.


Ok, that's an idea. I just don't want any of the sodium carb to react with the vinegar and end up adding unwanted elements to the final solution.
 
Nathanial.Dread
#127 Posted : 2/11/2015 2:35:08 AM

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I probably should remember this from Orgo II, but I can't seem to figure it out.

Hopefully this isn't too synth-y, I'm not trying to make anything weird (I promise), I'm just really curious about this question and like chemistry:

Does the amine in the indole ring of the tryptamine molecule behave like any other secondary amine, or does the aromaticity of indole protect it? If I'm doing some kind of reaction and want to target the primary amine on the end of the tail, would I have to worry about the same reaction messing with the indole amine?

Again, I'm really not looking to synthesize any drugs, this is purely a theoretic question from a chemistry geek.

Blessings
~ND
"There are many paths up the same mountain."

 
pitubo
#128 Posted : 2/11/2015 3:08:19 AM

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Nathanial.Dread wrote:
Does the amine in the indole ring of the tryptamine molecule behave like any other secondary amine, or does the aromaticity of indole protect it? If I'm doing some kind of reaction and want to target the primary amine on the end of the tail, would I have to worry about the same reaction messing with the indole amine?

This is not really "Basic chemistry" is it? AFAIK it is part of an aromatic system as you say yourself so it should be much more stable than the nitrogen on the ethyl tail. I'd say that unless you keep a jar of sodium amide in your cupboard then it should be unaffected by most forms of kitchen chemistry.

EDIT: very strong acids might protonate the indolic N, but again I assume that your not boiling in fuming hydrochloric acid in your kitchen.
 
Nathanial.Dread
#129 Posted : 6/13/2015 11:03:22 PM

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Still got questions Very happy

Does this seem viable?

Take plant matter (I was going to try ACRB and Chali both, just for experimentation sake), and soak in pure acetone for several weeks (4+), agitating occasionally. I was thinking that since acetone readily dissolves DMT salts and freebases, that there wouldn't be any need to acidify or basify the solution.

Afterwards, evap down on a baking dish, collect any residue, dissolve redissolve in acetone, and infuse into some kind of herb for smoking.

Any chemists here want to tell me if that won't work?
"There are many paths up the same mountain."

 
BongWizard
#130 Posted : 6/13/2015 11:50:48 PM

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You'll dissolve a lot of fats and tannins as well using acetone, although it is a viable method for liberating the DMT. You'd have to clean it up with a mini a/b to get crystals though. If you do try it, follow this quick method to clean up the acetone extract.

1) Dissolve the extract in hot naphtha or or non polar solvent of your choice (volume depend on how much extract you have, use the smallest amount that will dissolve all of it)
2) add an equal volume of warm vinegar to your nps solution, gently mix this over a period of 10-20 minutes
3) remove the acid layer and place in a flask that will hold 3x it's volume + 10%
Repeat steps 2 & 3 2 more times, giving you a total of 3 acid pulls with a volume 3x that of the original nps solution. This acid solution now contains your spice.
4) add NaOH (lye, caustic soda) or Na2CO3 (sodium carbonate, washing soda) in an amount sufficient to achieve a pH of about 12 (30g NaOH per litre of acid solution is more than sufficient) also, if using sodium carbonate, add very slowly to avoid overflow, as this neutralisation release CO2. You should notice the solution turn milky as the DMT becomes a freebase and comes out of solution
5) add 50mL hot naphtha to this alkaline solution and mix thoroughly (4 mixes and separations, you can shake it at this point without forming an emulsion)
6) remove the non polar layer (with a syringe/pippette or by careful decanting) and place in your evap dish
Repeat steps 5 and 6 three or 4 more times, or until no more DMT is visiblein the alkaline solution
7) evap the DMT laden nps to 10-20% of it original volume.
Cool freeze overnight
9) remove most of the nps and allow to thoroughly air dry

NOTE: this is all done in a warm (60-70C) water bath.

Alternatively, you could;
Dissolve extract in hot vinegar, give the gooey extract a good mix/fold with a stirring implement for 5-10 minute per pull (1x150mL per gram of expected yield plus 1x50mL per gram to ensure you've got everything). Next filter the vinegar mixture through a coffee filter to remove the insolubles (always pre wet your filter paper to avoid losing valuable spice solution which will be absorbed by the paper). Now, add 50 mL of hot naphtha and gently mix for 5-10 minutes to remove any fats/tannins that may have slipped through the filter. Remove the nps layer and discard. Now continue from step 4 above

That's just a quick run down of an easy acid base cleanup that can be complete in about an hour. If you have any more chemistry question or need any other advice, I am always happy to help.
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
Nathanial.Dread
#131 Posted : 6/13/2015 11:55:02 PM

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I'm not in a place where I can do much in the way of real kitchen chemistry, I'm looking for very low-tech, food-safe methods. The folks I live with are all good people, but some of them are uncomfortable around drugs, and I don't want to eat up a lot of kitchen space making them. Having naptha and measuring equipment would definitely raise some flags

Acetone has the benefit of basically being a tincture, so I can just say I'm doing herbalism stuff and it can all be kept in a jar, in my room, and then evaped over night on our deck.

I was thinking that egg-whites might work to gather up tannins? Or ideally, a vegan egg-white substitute. Alternately, maybe acidify with a little bit of vinegar and defat with cooking oil? This is the level of chemistry I'm sort of limited with.

Thanks though

Blessings
~ND
"There are many paths up the same mountain."

 
BongWizard
#132 Posted : 6/14/2015 1:32:45 AM

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I have heard that egg whites are a good option for gathering the tannins in a hot water mixture, although I'm not sure how it would work in acetone. It's worth a shot though. Cooking oil won't work for a defat (it'd actually be adding fat) but limonene (orange oil) will work for defatting and also in place of nps (although it doesn't evap cleanly, so using it as a pull solvent requires salting out). It's sold in Australia as a degreaser under the brand name OrganOil. So in your case, the best option might be to make a concentrate from acetone. Since most (if not all) of the goodies will be in salt form when directly extracted this way, you could then wash the fats and tannins out with limonene either directly or out of a mild vinegar solution (something like 1mL vinegar in 1L of water would be fine, this rate will give a pH around 5, you could go 1:10000 or even just use straight distilled water given that DMT will be 100% in salt form up to a pH of about 7.2). If I were you, I would probably go for a 1:10000 vinegar solution, just to be sure. Use a minimum of vinegar solution to suspend the gooey acetone extract (I'm talking tiny, just enough to get the goo mobile, because you'll have to evap this if you don't wanna do a two phase solvent extraction, although this has kinda become exactly that) and do a few defats with the limonene. When you're satisfied with the removal of fats/tannins, you'll wanna base the DMT, so now you'd add sodium carbonate to the point of saturation (somewhere slightly north of 450g/L from memory) and you'll see the dmt precipitate out as freebase. In a perfect world you could filter this and have crystals, but the world ain't perfect and your spice will absorb into the filter paper and you won't be able to scrape it up. Actually, scratch that! Duh! Filter this base mixture through a couple stacked coffee filters. Filter it again to make sure you've caught all your spice (filter another time if you feel it's necessary) and leave the filter to dry. Once dry you can extract the free base DMT from the filter paper using acetone (why that wasn't obvious to me to begin with is beyond me). Evap the acetone and you should be left with reasonably pure DMT freebase Big grin

It's worth mentioning that I haven't actually done this before (I'm more at home with dangerous toxic chemicals, after all) and it is, thus, just an exercise in theory, although I don't see any reason why it wouldn't work. Oh, it's worth mentioning that (given I found my head and realised you can wash the filters) you can use plenty of vinegar solution to suspend your goo (100mL le gram of expected yield is sufficient). Also, I realise this is probably getting a bit too involved for you circumstances, but remember, the extract can be done cold, you just have to leave extra time for the solvents to do their thing (adding a bit extra wouldn't hurt either).

Hope this helps. And as always, I'm here to help. Ask and ye shall be answered.
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
benzyme
#133 Posted : 6/14/2015 6:39:16 AM

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Nathanial.Dread wrote:
Still got questions Very happy

Does this seem viable?

Take plant matter (I was going to try ACRB and Chali both, just for experimentation sake), and soak in pure acetone for several weeks (4+), agitating occasionally. I was thinking that since acetone readily dissolves DMT salts and freebases, that there wouldn't be any need to acidify or basify the solution.

Afterwards, evap down on a baking dish, collect any residue, dissolve redissolve in acetone, and infuse into some kind of herb for smoking.

Any chemists here want to tell me if that won't work?



try ethyl acetate (non-acetone nail polish remover). dmt is more soluble in it.
to remove tannins, elute through activated carbon.

with a column, one could actually do an A/B extraction over amberlite IR-120.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
BongWizard
#134 Posted : 6/14/2015 11:09:59 AM

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Ahhhh benzyme Rolling eyes I think chromatography columns and amberlite are out of the question for this one. Not everyone has a fully equipped analytical lab at their disposal Laughing

Bit of a revision to the hypothetical method I explained earlier. So if you still don't wanna do a liquid-liquid extraction, you can forget about the limo and do it this way instead.

1) Dissolve your goo in warm vinegar solution, 100mL/g (expected). Really mix it up. Give it at least 15 minutes or so to pick up all the goods. During this 15 mins, give the goo at least 3 or 4 good mixes (shake it up if you've got it in a water tight container. You can add extra hot water to keep the temp up if needed.

2) Filter the vinegar extract through a few stacked coffee filters. This will remove most of the fats and other insolubles. Always pre wet your filter paper so as not to lose too much that might absorb into the filter. Squeeze all the moisture out of the filter then, briefly dip them in warm water and squeeze what comes out into your mix. Filter a couple more times (use a new filter for the second and third run ie one filter stack for the first run, one for 2,3,4 etc, so you should only require 2filter stacks total)

3) base the solution with sodium carbonate as described above (remember, go slow here). Now your freebase should come out of solution

4) filter the freebase out of the vinegar solution as described in my previous post. 3 filter stack, repeat 3+ times

5) once the filter have dried, soak them in acetone to remove the caked on DMT freebase, remembering to squeeze out all the solvent you can. As with the vinegar filters, dip in some fresh acetone and squeeze that into your DMT solution.

6) evap your acetone to reveal clean freebase DMT Big grin

So with that method, all you need is acetone, vinegar, sodium carbonate, warm water, a funnel, bunch of coffee filters and a couple jars.
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
benzyme
#135 Posted : 6/14/2015 3:30:14 PM

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BongWizard wrote:
Ahhhh benzyme Rolling eyes I think chromatography columns and amberlite are out of the question for this one. Not everyone has a fully equipped analytical lab at their disposal Laughing


Rolling eyes
don't need one.




$60 for the column, $65 for each bottle of resin. that's a living room.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
BongWizard
#136 Posted : 6/14/2015 3:49:53 PM

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Yeah, I know it's not overly expensive or difficult to source or setup. I've got a bit of a lab kit myself including several columns, condensers, a couple Buchners, all sorts of flasks, etc... Even proper bought a vacuum pump and a mag stirrer a while back (I know, not really impressive, but it made me feel special when I got them. Felt like a real deal lab rat lol) Alas, being on the road most of the time now, I don't get as much opportunity to play with them as I would like.

Anyway, my point was, I posted this proposed method because ND was looking for a decent cleanup using everyday household chems. Much to my dismay I found this thread by endlessness not an hour later Sad

https://www.dmt-nexus.me...aspx?g=posts&t=30501

My method is slightly different, but the essence is the same; an extraction where the chem supply cupboard is under the kitchen sink Big grin
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
benzyme
#137 Posted : 6/14/2015 4:34:22 PM

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there are many, many different ways of applying the art.
I mention the column because it is a simple, one container solution.

my preferred method: sonicate in dilute vinegar, filter, basify, extract, rotavap. the 1 hr. tek.
i've also suggested the presto (pressure cooker) method. no matter what acids/bases and solvents are used, first priority should
be plant cell lysis.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
BongWizard
#138 Posted : 6/14/2015 6:38:43 PM

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That's what I love about chemistry. So many ways to the same right answer, though in this case, every method is really just a slight twist on the last.

Mmmmmm, sonicator. I would love to own one of those bad boys. Would make everything so much quicker and easier. Just out of interest, what's your favourite (or, in your opinion, the best, if you don't like playing favourites) non polar solvent for DMT extraction from bark?

Personally I use much the same method (less the sonicator and rotavap, obviously) except I like 0.01M HCl for the acid phase. As for solvents, I like to do my first extract with xylenes then naphtha for the second base phase (only because, you wind up with a net cost saving based on Aussie prices). Usually takes ~2.5h + evap time, because I like to leave the bark under acid for a bit longer (seems to be the biggest factor influencing yield in my case).
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
benzyme
#139 Posted : 6/14/2015 6:43:36 PM

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favorite? methylene chloride.
soon to be favorite: supercritical CO2.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
BongWizard
#140 Posted : 6/14/2015 8:19:40 PM

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Of course... DCM... Yeah that is a good one. Thumbs up

Supercritical CO2 sounds interesting. I briefly read the thread regarding it (must remember to go over it more thoroughly). Seems like a really efficient method of DMT extraction if coupled with the right hydrocarbon solvent. I'm interested to see how this works for you. Have you got an extraction vessel yet? My only concern is in using an open system. Have you figured out how much SC CO2 you will get from your cylinder before the pressure is below the critical point? A closed system is much more expensive to build, but I think you'll find yourself running to the welding store rather often. As always, just my thinking, correct me it I'm wrong
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
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