Introduction and first mistake!

[Bdust]

Hi all!

First of all, I would like to thank this entire community, as it is incredible to be able to acquire all this knowledge from peers... 20 years ago this would be a dream...

So, as the title mentions, I tried my first extract the other day, and unfortunately had bad results.Using Cybs tek, temps were a little high at all stages (~70 C), but had no precipitation at freezing. I believe to have found the culprit in the Naphtha I have, which is C9, aromatic naphtha (CASs 64742-95-6 I believe). After a little reading, I have heard this would have dissolved the dmt, but would not precipitate well in the freezer? So I guess I have 3 questions that someone may be able to help with:

1. Could my assumption above be correct, or should I re-evaluate my process and see if anything else could have gone wrong? (i.e. I Ph´d to 3 first, then to 14, so I know these values should be correct?)
2. Could I potentially (And as a fun experiment), recover the dmt from the naphtha by means of an acid wash? Would this involve using an acid, and doing some washes and pulls, which I could then basify and re-extract?
3. I can acquire some Heptane, as I can not find any other suitable naphtha (EU) (Well, another called Nafta 16/18 S-100, CAS 95-63-6, but little faith?). Would this be a suitable replacement? I can also get Toluene, or Hexane, would this be better?


Many thanks in advance for reading this post, and if it should live in another place, please let me know!

 

[Physics131]

Hi and welcome.

I think that 70°C is somewhat the higher temp edge.
Did all myextracts with that temp and I think that the higher the temp the more yellow/orange the yield gets.

Regarding 1. i do not know.

Regarding 2. you could do a backsalt if you want. As you already said washing it with acid water. That acid water would pull the dmt from solvent to water. Then seperate the solvent from the water. Add lye to the acid water. Then make your pulls with a different solvent.
I would make an evap test. If your solvent evaps clear it should be ok.
Also there are solvents which should not be used, I am unsure about yours.

Regarding 3. Heptane works well, I think some also used Tolune or Hexane but I would use the forum search funktion to double check that.

IMO i would backsalt it and pull with Heptane.

 

[Bdust]

Hi and welcome.

I think that 70°C is somewhat the higher temp edge.
[...]

Many thanks!

This is exactely the info I needed! The term backsalt was missing from my vocab and has opened a world of info...

Perfect, I guess I will experiment with backsalting and heptane, and this will confirm if my assumptions on point 1 were correct!

Thanks again!

 

[Bas Sarkin]

Hi @Bdust, welcome!

I would steer away from your current solvent. I am far from a proper chemist, so someone correct me if I am wrong, but I think 'aromatic' means 'circular' which means 'no good', think benzene. I want my carbohydrates straight or branched, but not circular.

Here is a fact sheet about CAS-nr: 64742-95-6 note: Carcinogenic & Mutagenic
Then there is this pdf, that confirms its carcinogenic properties, and also shows the lethal doses for mice etc. Get 0.3 grams of this in a 100kg body, and you have 50 percent chance of dying, it seems (LD50 means lethal dose for 50 percent).

I think in Europe you can order Heptane just fine, about 10 euro/L, I personally like Coleman's Fuel, CAS-nr: 64742-49-0 (pdf), its cheap and readily available locally for me.

Also: I don't know if you followed the tek to the letter, but if you use lots and lots of naphtha on a small batch of plant material, it might all stay dissolved when in the freezer. Say you did 10 grams of MHRB, you would expect +/- 0.1 grams of DMT out of that, and perhaps you used 100 ml of naphtha to pull it, it would all stay dissolved (rule of thumb is roughly 1 mg dmt in 1 ml of naphtha at -20C, 30mg per ml at 20C).

 

[pantostao]

My first extraction used C9 naphtha as well. I found that:
- It dissolves DMT really well
- It isn't suitable for freeze precipitation

At this point, you can recover the DMT out of the solvent in one of these two ways:

1.- Backsalting. Add acid to your solvent so DMT salts crash out and then recover in other ways. Read on FASA/FASI/FASW on this forum, there is lots of info.
I have never done this, but I believe it should work. This would be the clean way.

2.- Evaporate the solvent completely. You should only do this if you're certain that your solvent is pure enough. Industrial solvents are not. Did you do a evaporation test on it?

 

[Bdust]

Hi @Bdust, welcome!

[...]

Many thanks for this detailed answer! I will be getting rid of this solvent!!

I have gone ahead and got some heptane, which at least I know is a single component (Vs mix) and should work, I may also experiment with Coleman's fuel (or similar), thank you very much for putting a CAS reference number in there, it is so useful...


Thank you for your detailed response, I will out it to good use!
(I did follow the recipe with 50gr of MHRB)

 

[Bdust]

My first extraction used C9 naphtha as well. [...]

Many thanks for this answer!!

It gives me some reassurance that this was in fact my mistake...

Many thanks for the backsalting tips, this is a term and process I did not know and need to read on this, sounds like fun!

Thanks again for your experienced answer, it gives me some nice reassurance!

 

[Bdust]

Just wanted to put a quick update here, and let you all know that your invaluable knowledge has led me into a beautiful extraction of white beauties!