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My first extraction (STB): success and freebasing problem Options
 
karloff
#1 Posted : 8/28/2016 10:29:06 PM

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Hi!
I have been learning from DMT-Nexus for more than a year now. This weekend, finally, I made my first extraction. I tried a STB method, pulling with limonene and using FASW to extract the DMT fumarate.
I used a magnetic stirrer for mixing well before each pull and I think that helped to achieve an excellent yield: 1,5 gr. DMT fumarate from 80 gr. MHRB.

Many thanks to all the people that has collaborated on this site and developed the techniques that have made things much easier for begginers like me.
This is a photo of my final product:



But now I am asking for some help, because, after finishing the extraction without any problem, I think I have made a mistake when I tried to do freebasing of the spice.

I wanted to freebase one half of the product: 750 mg.
So, I mixed it with 750 mg. of sodium carbonate.
Then, I added 30 ml. of distilled water and stirrer in the hope that the DMT freebase would precipitate away, because it is not water soluble.
But only a tiny bit precipitated, like a drop of yellow honey, the rest is white liquid.

Reading again the techniques, I think my mistake has been to add so much water, that disolved the fumarate before it reacted with the sodium carbonate... Is this right?

I should have used 1-2 ml. of water as much.
Now I have this mix slowly evaporating, but I am not sure what to do with the solid stuff I will obtain.... please, how can I save my DMT and get it finally freebased?
Many thanks in advance
 

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hermes111
#2 Posted : 8/28/2016 11:01:55 PM
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Hi & congratulations Smile.

It's better to pre-dissolve your fumarate and then add the sodium carbonate powder or better solution. The reaction is supposed to happen in solution.

Add a little more sodium carbonate to the liquid and put it in the fridge overnight.
It's hard to judge the amount that's in a freshly participated solution since the particles are so tiny(especially if you use a magnetic stirrer), the more water you use the less you see. Be patient and don't throw the original solution away too early, if you put the solution in another container and let it sit some more after your main batch, you'll often come back to find some more fine dust settled.

The yellow oil might be impurities from your limo and/or DMT if your solution got too hot (adding sodium carbonate to water is slightly exothermic, that's why for that application it's usually pre-dissolved, DMT melts easily)

Don't underestimate how much DMT there can be in a little drop of oil, that's the densest state DMT can be in. When crystallizing a thin layer of oil, you'll often see the DMT 'blooming' and developing a thick crust of crystals over the oil.

Just let the oil stand around and scrape it occasionally and it should crystallize Smile.

Edit: Sorry overread the last part. Don't evaporte to dryness with heat, you might lose product. Just evaporate it to an easily handled amount. You can just start from scratch by putting white distilled vinegar in your solution (careful, bubbles and foaming) until it stops reacting, and add some extra, and then rebasify with sodium carbonate(room temperature solution). No need to be exact, adding too much is better than too little. Putting it in the fridge after you're done helps with precipitation.
 
karloff
#3 Posted : 8/29/2016 8:22:04 AM

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Many thanks hermes111

What you say makes sense: I have got up in the morning today and took a look at how the evaporation was going. To my surprise, there were some white spots at the bottom of the container. I was not sure if it was DMT or sodium carbonate, but after reading you I think it is DMT freebase that has started to precipitate.

Now I am at work, but I will follow your advices when I get back home. But let me confirm that I have understood you well (because English is not my native language):

What I will do is to add some more sodium carbonate (let's say 500 mg.?), stir a bit and put it in the fridge (not freezer). Then wait for new precipitations at the bottom.
These are my doubts:

1) ¿Should I add some more water too?

2) ¿Could I bring out the current white spots before adding the carbonate?

3) ¿Can I bring out the new precipitations as they go forming, or is it better to wait for all the precipitations to be finished?

3) ¿Will I obtain all the dmt freebase by this method?

Many thanks in advance!
 
hermes111
#4 Posted : 8/29/2016 7:45:14 PM
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No problem.

That's likely DMT. The only way you will see sodium carbonate crashing out of water, is when you have prepared a supersaturated solution (dissolving as much sodium carbonate in water as possible when the water is boiling, and filtering it afterwards) and it cools down too much. You can always test if it's DMT freebase or sodium carbonate by trying to dissolve it in dest. water. DMT won't dissolve, sodium carbonate will very easily in cold water.

Your english is just fine Smile. Yes you can do that exactly, but then you'll have to wait for the oil to crystallize. To get a nice uniform product it would be better to start from scratch and add vinegar & rebasify. But it really doesn't matter that much.
As I said the exact amount sodium carbonate doesn't matter much. Too much is better than too little, I'd just add about a quarter teaspoon. And if you think you've added too much, you can always even things out by adding more water.

1) You can but you don't have to. 30mL is more than enough to work with in this case. Depends how big your container is. Keep in mind the wider your container is, the more it is going to look like you don't have much material.

2) You can easily separate everything that is at the bottom of the solution. It's going to slightly stick to the bottom, so you can just pour out the solution into another container.
But you don't have to, adding more sodium carbonate to it will not affect the already precipitated DMT, except if it's very hot (will melt).

3) See 2), as I said you can pour the solution carefully into another container & keep what sticks to the bottom first, and let the solution settle again. But I usually just wait overnight to harvest my main precipitated batch, and another day to get everything that precipiates afterwards.

4) I'm not sure if it's exactly 100%. But the majority, yes.

You're welcome & much success. Don't throw your solution away until you're sure you've got everything out Razz.

 
karloff
#5 Posted : 8/30/2016 8:29:25 AM

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Many thanks Hermes, I really appreciate your comments.
Finally the conversion proccess seemed to be right, but I did not expect the product to be so oily, so I made a big mistake: I threw away the first precipitates that got stuck to the scraper I was using for stirring (I though it was limonene traces or something). My stupid error!

Anyway, your comments clarified things a lot, so I started to collect all the other oils that precipitated at the bottom of the recipient. Adding more sodium carbonate didnt' make more precipitates, but I am keeping the solution (in evaporation proccess) following your advices to see if I can somehow milk it a bit more.
This is how it looked:



I left it drying overnight and, as expected, it become a waxy paste that was not difficult to crush a bit:



This weights a bit more than 300 mg. I think it would have been 500+ mg. if I had not thrown away the first oils, but at least I have learned a good lesson Big grin

I have left it drying some hours more, but I will definitely store it as soon as I get back home after work, to avoid too much oxidation. I hope I will do my first vaporization tonight.

May thanks for your help, it has been greatly useful.
 
hermes111
#6 Posted : 8/30/2016 9:20:18 AM
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Good job mate Smile. I warned you not to throw anything away haha.
But don't worry too much about it, many of us including me yielded nothing or very little material our first time. Do it once or twice again and it will become second nature.

No urgency to remove your DMT from air, for longterm storage that's best, but it won't degrade your material if you don't do it tomorrow.

Happy travels and take care.
 
karloff
#7 Posted : 8/30/2016 9:07:59 PM

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Confirmed: the product is super-potent when vaporized Very happy

Thank you again for all your support hermes111, Thumbs up
 
 
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