Extraction questions

[Trev_sunyata]

Do I understand this right? naphtha and heptane won't pick up up dmt n-oxide, but when I dry my crystals and they turn yellow, that's probably n-oxide forming, so if I save up all this then re-x, am I losing a decent amount of yeild?

If I like n-oxide in the mix, would it be ok to just do an extra socarb wash on them then evap most of the way and freeze percipitate?

If it's really important to do a re-x then, can I put all the goop left behind into the basic mix then pull with a full spec like d-lim, salt it, add zinc to convert to n,n dmt then filter and re pull

Either way I'm going to try the salt and conversation on my stuff because my bark is very old and I'm sure there is a lot of n-oxide in it

 

[downwardsfromzero]

There's no direct evidence that the yellow coloration is due to N-oxide formation. Nor is there any evidence that N-oxide formation occurs in old bark. There's a good thread, stickied, that discusses the colour of DMT and how it's not altogether important if it's orange, yellow or white. (Black, blue or green is another matter entirely!)

The material that provides the yellow-orange discolouration is very intensely coloured and thus is present in minuscule quantities. Whether you want to clean it up is of course entirely up to you but bear in mind that sodcarb washes are notorious for reducing yield and you can make a fair bet that your material recovery after a zinc reduction won't be 100%. And what's to say when you dry your crystals again after all this fiddling about they won't simply turn yellow all over again?

During a hot recrystallisation process with naphtha or heptane, an orange-brown oil will separate at the bottom of the container, from which the clear-to-yellowish naphtha can be separated. The remaining orange oil will also solidify (sometimes it takes a while) and analysis has shown it still to consist very largely of DMT.

I'm all in favour of tinkering and learning about stuff, but if your priority is good yields prepare to be disappointed and/or frustrated.

 

[Trev_sunyata]

I don't mind the yellow at all, I was trying to say that I want to keep it but was worried that further processing would cause loss of it.

I don't think the socarb wash will result in much loss, the freebase alkaloids aren't going to go back to water soluble forms without dropping the pH. I tried to only pick up the water to discard, leaving any goo or precipitated crystals between the layers. When getting to the end of the dropper, there is that last drop that is half water, half solvent, but I guess I'm just going to hope not much was lost there.

Thanks for info on n-oxide and it's non confirmed formation. I had read that thread about color and am fine with smoking colored spice as long as it isn't too sticky which mine was completely dry. I just noticed that some of it would not redissolve in naphtha, turned into a goo at the bottom of the solvent, this wasn't the case before it's evaporation and being left under the fan too long.

I just did that second socarb wash and am going to not do a heptane re-x. So that I can keep the suspected n-oxide with it.
I am still going to try a full spec pull with salting then zinc on my basic soup to see what happens.
I added some more lye and am trying one more pull to make sure I got everything before attempting it.

 

[downwardsfromzero]

Bear in mind that some have claimed the purported N-oxide is more potent anyhow. A disadvantage might be its oily texture.

Sometimes DMT crystals are just yellow anyhow, probably due to polymorphism.

Have fun with any tinkering! Keep an untreated reference sample if you do the zinc reduction, just to see if it actually does anything. Pics and lab reports are most welcome here

 

[Trev_sunyata]

Have fun with any tinkering! Keep an untreated reference sample if you do the zinc reduction, just to see if it actually does anything. Pics and lab reports are most welcome here

What do you mean about the reference sample?
Do you mean when I do the full spectrum pull, and after salting, save the left over non-polar to evap and re-x to see if anything is caught, then set some of the polar solution to the side to evap before adding the zinc to the rest and continuing that process?

 

[downwardsfromzero]

Keep a reference sample from the salted DMT before treating the rest of it with zinc. So yes, set a little of the polar solution to the side. The NPS can be saved for solvent recycling/reuse.

 

[Trev_sunyata]

Wow, I have not done the full spectrum extract yet, but I did just freeze percipitation everything, had 0.15 in small crystals from 2 other pulls, this time I took the latest pull, evaped down, poured it over the already dried spice and stuck in the freezer, now I have yellow see urchins covered in swords! They look so cool, I have gotten small pin-needle groupings but these have mass in the middle and the crystals fan out like swords, most of them look near a quarter inch high.
They are not dry fully though, I don't think. Still have to pull them off the glass but there is a bit of still sticky looking yellow goo spots around them. Not sure of my yeild in weight but these look so big compared to the amount of small scrapings I poured the newer solvent over.

Is it ideal though to ground and mix everything up in there and leave to dry more?
I may just keep the crystals separate and put all the jungle spice that's coming next together, but in the end I may just dissolve everything on changa.