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Reddish Naphtha after A/B extraction Options
 
mercurio
#1 Posted : 5/19/2011 1:45:10 PM
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Hi,

I "condensed" 6.5 Kg of bark into a very dense liquid (about 2 liters) after boiling it three times and then simmering the lot for evaporation.

Q1: am I pushing it too much? Shall I evaporate it to a little more? That is, did I make it too dense?

I then added lye (Caustic Soda) to the mix till it reached PH 14. Then added naphtha, shook it well (with rest periods to maximise yield I hear) and then, when they separated (letting it rest for a good 1/2 hour), I took the naphtha out. I didn't use much in the first pull -- I used to use a lot, and got told off in these forums!)

Well, man, it was red. Like red-red. I noticed that the bark I used had a really strong red colour, and it was really fresh.

Q2: Gosh... why would it come out so red? Is it even "normal"? Was it because the liquid was too dense to start with?

I am in the middle of my extraction right now, and would love to figure out what to do. Shall I continue? Or did I do something terribly wrong and should just give up?

Q3: If I do continue (I am now in the middle of the second pull), shall I just wash the crystals afterwards?

That's it!

Thanks a billion as ever... Very happy

Mercurio


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endlessness
#2 Posted : 5/19/2011 2:06:02 PM

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The first thing that would call our attention is the amount you are extracting. 6.5kg?! I mean, I dont want to accuse you of anything, but you must understand the first thing that comes to my mind is that you might be selling it, and as you can see in our FAQ and attitude and so on, we are extremely against selling of DMT.. Even if you are not selling but just giving it away, it is so much DMT that it makes me wonder if you are giving it in a personalized way, carefuly introducing each person, or if you are giving big quantities away in ways that can be potentially dangerous. So, are you selling it or giving it away indiscriminately/recklessly? If so, please for the love of god reconsider what you are doing (and check all the reasons in the thread linked in the FAQ why we are against selling dmt)

Also it makes me wonder, how comes you are asking these things and dont know them, but are already extracting such large quantities?

Now, as for red naphtha, check the FAQ. My suggestion is resalt with vinegar 3x, re-base that vinegar and re-extract. Or in the very least doing a sodium carbonate wash (not of the crystals, of the solvent!), freezing your solvent and doing recrystallization if necessary. Yes it could very well be that because of how dense it is, small suspended particles of the acidified layer came across and refuse to settle, or something of the sort. Doing this mini-a/b with it should clean it up. Good luck (hoping you are not having any profit/'cold-trade' intentions)
 
mercurio
#3 Posted : 5/19/2011 2:08:00 PM
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Hi,

Good news!
The second pull has a colour I am *much* more accustomed to -- and it's really quite yellow!
I think I will give this one 4 pulls, seeing how much bark there was.

Have a look at the two pulls... I still don't get it.

SO, I guess the question is: how do I clean that first pull?

(Right now, it's a disgrace!)

Merc.
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mercurio
#4 Posted : 5/19/2011 2:20:53 PM
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Hi,

Where I am, there would be nobody willing to buy it, and no need to introducing it to anybody since _lots_ of people know what it is...
This is my third attempt -- the first two, I had very low yields. I am a *little* sick of extracting, and this time I really want to get it right.
Before your post, I didn't even realise that I was actually working on a huge amount...
So... Not selling it -- I want to extract about 10 grams, and basically never extract again.

(You can read my failed, lame previous attempts in these forums. Plus, I am about to go for a big trip)

Anyhow.

My lame-ness also means that I am having trouble following you. I know what you mean by "My suggestion is resalt with vinegar 3x, re-base that vinegar and re-extract." -- if anything, because it's the last step explained in the lex tek (right?).

But... how do you actually do a sodium carbonate wash? What is recristalisation *exactly*?

Any pointers would be awesome...

I am still wondering why this happened... ugh. I really wanted this one to be a good attempt, and... meh.

Bye!

Mercurio

endlessness wrote:
The first thing that would call our attention is the amount you are extracting. 6.5kg?! I mean, I dont want to accuse you of anything, but you must understand the first thing that comes to my mind is that you might be selling it, and as you can see in our FAQ and attitude and so on, we are extremely against selling of DMT.. Even if you are not selling but just giving it away, it is so much DMT that it makes me wonder if you are giving it in a personalized way, carefuly introducing each person, or if you are giving big quantities away in ways that can be potentially dangerous. So, are you selling it or giving it away indiscriminately/recklessly? If so, please for the love of god reconsider what you are doing (and check all the reasons in the thread linked in the FAQ why we are against selling dmt)

Also it makes me wonder, how comes you are asking these things and dont know them, but are already extracting such large quantities?

Now, as for red naphtha, check the FAQ. My suggestion is resalt with vinegar 3x, re-base that vinegar and re-extract. Or in the very least doing a sodium carbonate wash (not of the crystals, of the solvent!), freezing your solvent and doing recrystallization if necessary. Yes it could very well be that because of how dense it is, small suspended particles of the acidified layer came across and refuse to settle, or something of the sort. Doing this mini-a/b with it should clean it up. Good luck (hoping you are not having any profit/'cold-trade' intentions)

 
endlessness
#5 Posted : 5/19/2011 2:31:11 PM

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I suggest you read the FAQ, it should explain a lot of things you are asking.

Typically from good sources people have been getting anywhere between 0.8-2% dmt, so 6.5kgs with good bark should yield you 50-120g dmt, not 10. Thats DMT enough for the lifetime of an army (so now you see why it sounds so absurd) Razz

If your yields are bad you should question your bark source, to begin with. Check our suppliers section for good reviews.

Please check the FAQ about wash and recrystallization, as well as general extraction tips and overviews and links therein, and if after reading it all you dont understand something, feel free to ask

And no the last step in lextek is freeze precipitation. What I mean is, instead of freezing your dark solvent, you mix it with vinegar 3x, which will pull your alkaloids again to the vinegar. Then you add the base to that vinegar, add clean solvent and do another 3 pulls, then evap or freeze as you would normally. Makes more sense? Read FAQ and a couple more teks to get the idea and come back Smile
 
mercurio
#6 Posted : 5/19/2011 2:38:40 PM
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Hi,

Err... excuse me?
Are you really telling me that I will get 90g of DMT from this?
Ah, now it's a _little_ clearer on why the previous poster was wondering about me selling it. In fact, god knows *what* I am going to do with all this DMT.
I really had no idea. I mean... meh. I don't even know what to say.

If you know that Tek, I actually meant the part called "Part 5: Defat Step 1: Acid Wash"... is that what you are talking about?

Bye!

Mercurio
 
endlessness
#7 Posted : 5/19/2011 2:43:48 PM

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nope thats not what Im talking about... Smile
 
Enoon
#8 Posted : 5/19/2011 2:49:29 PM

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what I like to do with red naphtha, and this works very well, is:

1. freeze it for about 20 minutes (might vary depending on the temp of your freezer)
2. there will be gunk at the bottom of a new more clear liquid - so decant but keep both
3. the liquid goes back into the freezer for freeze precipitation, the gunk has to dry completely (this takes about 1.5 days maybe)
4. use anhydrous acetone or IPA to perform a *pull* on the gunk / repeat two or three times, filter the IPA through coffee filters and put in an evap dish.
5. let the ipa evap and you should get a waxy residue which is dmt.
6. scrape the wax, cut it up, let it dry... enjoy
7. don't forget the naphtha in the freezer which should by now have precipitated some crystals.

if you are lazy you can just freeze the red liquid for a longer time. then you will have crystals and gunk at the bottom of your jar together. You can pull these just as I described with the gunk alone too. lately I prefer this more lazy approach.
the result is nummy but it does lack the pretty crystal structure. I do think the more amorphous dmt somehow melts better in the gvg and thus works better for vaping. I could be wrong though.

anyway... dude 6.5 kg?!!!? make sure you store your results well so they don't go bad. would be a shame to waste so much.
and if you yield less than what end suggested... keep going. don't throw it out!!

Buon viso a cattivo gioco!
---
The Open Hyperspace Traveler Handbook - A handbook for the safe and responsible use of entheogens.
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mushroom-grow-help ::: energy conserving caapi extraction
 
mercurio
#9 Posted : 5/19/2011 3:06:35 PM
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Hi,

I didn't even know DMT would go bad!

Hey I am at my third pull, the two layers are in a tall jar, in a pot of really warm water, and guess what? It won't bloody separate. It's so hot in this room, I am sweatting with not t-shirt on.

What do you do when you get a non-separation event? Do you have a fantastic solution for that too?

Everything seems to be going wrong, except for pull n. 2!

Mercurio
 
endlessness
#10 Posted : 5/19/2011 3:15:24 PM

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FAQ again Smile
 
mercurio
#11 Posted : 5/19/2011 3:17:37 PM
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Hi,

Just found it, IDIOT ME!

The layers wont separate, what to do?

Possible fixes:

Dont shake next time, if you did so! Instead, Stir/roll/turn upside down slowly, several times.
Add more basic water/lye to the mix (either mix is not basic enough or too much plant matter for too little water)
Make a warm water bath with the whole container (remember no fire sources near solvents, and leave top slightly open for preventing building up of pressure)
Tapping on the side of the container/vibration (like sitting on top of washing mashine)
Adding plenty of no-additives non-iodized salt (will make the water more polar and therefore chemically help in the separation)

Mercurio
 
mercurio
#12 Posted : 5/19/2011 3:44:02 PM
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Hi Endlessness,

I read the FAQ.
However, I am still a little confused.
You wrote:

And no the last step in lextek is freeze precipitation. What I mean is, instead of freezing your dark solvent, you mix it with vinegar 3x, which will pull your alkaloids again to the vinegar. Then you add the base to that vinegar, add clean solvent and do another 3 pulls, then evap or freeze as you would normally.



I asked:

> If you know that Tek, I actually meant the part called "Part 5: Defat Step 1: Acid Wash"... is that what you are talking about?


You answered that that wasn't it.
But!

It really looks like it is...


From the tech:

1. Again, acidify an
excess amount of
distilled water by
mixing one part
vinegar to three parts
water. You are aiming
for a pH of 4.
Use a digital pH meter
or litmus paper to
determine the pH of
the solution.

2. Add approximately
250mL of acidic water
to the Shellite solution.
The mixture does not
need to be hot; in fact
it is better if all liquids
at this step are kept at
room temperature as
otherwise plant gunk
will come back across.

3. Using the same
siphoning method in
Part 4 - Step 3, siphon
off the top non-polar
layer from the bottom
polar layer, this time
keeping the polar layer
(acidic water).


3. Repeat step 2
three more times
and combine the
three polar layers.
For the third time
use 500mL.

(That's the vinega pulls you talked about, right...?)

And then:

1. Slowly add 60 grams of
Sodium Hydroxide to the
solution to raise the pH to 14.


And then you pull it again 3x with the naphtha.

Isn't that it?

Mercurio
 
mercurio
#13 Posted : 5/19/2011 3:46:21 PM
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Hi,

Plus, I have tons of crystals forming *right now* at the bottom of that naphtha at *room* temperature...?!?

Mercurio
 
endlessness
#14 Posted : 5/19/2011 3:53:28 PM

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Im sorry I had read it wrong, thats pretty much the process yess.. Usually defat just means mix the solvent with the acidic solution before you basify at all in the first place, but youre right what you described is what I meant

tons of crystals is because there is so much damn dmt there (lol ) that the solvent is supersaturated and therefore its starting to crystalize. If you stick in the freezer you'll have a massive amount of crystals for sure. Which pull is it crystallizng at room temperature, the red naphtha one or the other clearer one? If its the red naphtha, I would suggest doing the clean up anyways, as soon as you add the vinegar it will dissolve in the vinegar. If its the clearer one, just stick in freezer for a few hours
 
mercurio
#15 Posted : 5/19/2011 3:59:26 PM
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Hi,

OMG I put acidic water (PH 3.2) in it, and the crystals *just* *won't* *desolve*...
They are all sitting at the top... this needs a photo.

Mercurio

endlessness wrote:
Im sorry I had read it wrong, thats pretty much the process yess.. Usually defat just means mix the solvent with the acidic solution before you basify at all in the first place, but youre right what you described is what I meant

tons of crystals is because there is so much damn dmt there (lol ) that the solvent is supersaturated and therefore its starting to crystalize. If you stick in the freezer you'll have a massive amount of crystals for sure. Which pull is it crystallizng at room temperature, the red naphtha one or the other clearer one? If its the red naphtha, I would suggest doing the clean up anyways, as soon as you add the vinegar it will dissolve in the vinegar. If its the clearer one, just stick in freezer for a few hours

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endlessness
#16 Posted : 5/19/2011 4:08:04 PM

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Did you just pour it in or did you mix well? Insist on mixing, they should dissolve.. Or separate the acidified water you added, and add more fresh acidified water, but make sure its hot/warm acidified water. It should def dissolve after insisting a bit

Keep us informed, dont throw anything away and dont worry it will be saved Smile
 
mercurio
#17 Posted : 5/19/2011 4:19:50 PM
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Hi,

I am not going to mention the crystals that I spilled on the table by accident while using a paper funnel.

What I am going to mention, is that I am now re-separating with the acidic water. My goodness, everything three more times!

In the meantime, the third pull -- the one that won't separate. That's an interesting one. I added more lye, and I added more naphtha as well.
They are _slowly_ separating -- how long shall I wait? The third bullet here is the salt... and I only have salt with anti-caking agent 535. What shall I do?

Mercurio
 
mercurio
#18 Posted : 5/19/2011 4:24:07 PM
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Hi there,

DO colours look right?
Is this ready for me to take the bottom bit out?

Bye,

Merc.
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mercurio
#19 Posted : 5/19/2011 4:25:24 PM
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Hi,

Plus... why do you think the bottom layer is this pink...?
Is that normal?

Mercurio
 
endlessness
#20 Posted : 5/19/2011 4:28:54 PM

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yeah seems you can take it out, the crystals dissolved now I guess? Its pink because it has carried the polar impurities that were suspended in your naphtha. Now base and extract, dont shake but rather stir when you mix the solvent to the based solution, and it should all work

I would say do at least 2 vinegar pulls on that solvent, and then do at least 3 naphtha pulls on that vinegar solution after you pull it.

Oh and btw, considering something you said in some posts back.. You said you think you will do 4 pulls total to the main mimosa container? Definitely do more! Do at least 5-6 pulls, and the last one, you leave it for long, like a day or two, occasionally stirring it. Then freeze that last pull separately, and if you still have a significant amount of crystals coming out, do more pulls Smile
 
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