Tips for first timers from SWIM's first time and a Q re: freeze precip

[triptatmos]

So SWIM has just taken all his pulls from his first attempt and wanted to share some little advice as he had done lots of reading and still made some mistakes. SWIM hopes his mistakes will help improve others first attempts.

SWIM chose to do a modified version of Noman's Tek. 50g powdered, 750ml water, 55g lye & 60ml naphtha (per pull).

SWIM chose to use a pickle jar - DO NOT DO THIS unless for very big pulls. The width of the 2.25 litre jar made the layer of naphtha very thin. Forget about trying to have ample space and get a thinner container. However, SWIM decanted the difficult last parts into a measuring cylinder and it was a good way around this.

Also SWIM thinks 60ml of naphtha was possibly too much per pull, so don't be afraid to go a little under and have a few more pulls.

NOW THE QUICK QUESTION:

SWIM thinks that he didn't evap enough naphtha off his first few pulls before doing his freeze precip. There was cloudy stuff forming on top when blown on, but possibly was too saturated. SWIM doesn't want to lose any of the goodies so is wondering whether when he pours off the naphtha to collect the crystals if he can evap the naphtha some more a try get more crystals. SWIM thinks this is correct, but from his research is a little confused whether it needs to be returned to the soup first.

SWIM also wants to say thank you to everyone who has been so helpful in sharing this brilliant information to the world. SWIM hopes that his little info can help someone else on their journey.

 

[downwardsfromzero]

Tip for first timers: the water is shallow, no need to swim here

[...] thinks that he didn't evap enough naphtha off his first few pulls before doing his freeze precip. There was cloudy stuff forming on top when blown on, but possibly was too saturated.

This doesn't make sense. If there wasn't enough naphtha evaporated off, there's no way it could be too saturated. If it were "too saturated", the DMT would start crystallising before it got anywhere near the refrigerator, let alone the freezer. As you already note, just use smaller amounts of naphtha for each pull. That alone will ensure each pull is more concentrated so that you won't have to evaporate any naphtha.

[I don't] want to lose any of the goodies so [I'm] wondering whether when [I pour] off the naphtha to collect the crystals if[ I] can evap the naphtha some more a try get more crystals. [I think] this is correct, but from [my] research [I'm] a little confused whether it needs to be returned to the soup first.

There is no need to evaporate. While the base soup has been sitting more DMT will have been released from the bark, so re-use the naphtha in 30 to 40 mL portions to do more (about 3) pulls on the base soup. Try to do these pulls at about 40°C. These can then be combined and put in the freezer to precipitate again.

Once the base soup appears to be exhausted and the naphtha has come back out of the freezer, you can perform a mini A/B on all your used naphtha. The DMT gets extracted back out of the naphtha into a few small portions of vinegar. This vinegar can then be evaporated down, mixed with a suitable amount of base and pulled again with a small amount of solvent of your choice. Sodium carbonate and acetone are pretty good for this last step. Acetone evaporates very easily, although you can use naphtha again and do another tiny freeze precip - potentially repeating ad infinitum

It's also worth noting that if you leave the naphtha-pulled base soup sitting (covered!) for a couple of months, the remaining trapped naphtha floats to the surface and slowly evaporates, leaving solid DMT floating on the surface. Of course, you need a safe and secure location for the frankly hazardous base soup to be stored in order to observe this effect, which gives an indication of just how thorough the initial pulls were.

 

[triptatmos]

Thanks for the reply. Yeah sorry about that I made a mistake I meant not saturated enough. Whoops! Basically, think I used too much naphtha and didn't let it become more concentrated before freeze precipitating as I read that this can reduce yields.

To note: Bark and lye was left for 12 hours before, then three pulls were combined in one tray - this is the one which might have too much solvent, so I fear that it might effect yields. Then a final one pull sat for 24 hours and was stored separately, this seemed to go well - instantly cloudy.

Thanks for the A/B tip. Am I right in thinking that this is for the naphtha that may still contain a little bit due to the freeze precip not catching it all?

Would it also be possible to simply just try evap this remaining naphtha to see if any more goodies appear? It seems to me less complex than another procedure.

But will give the A/B tip a go. Much appreciated!

 

[downwardsfromzero]

Evaporation is a simple way of recovering the goods, but then the solvent is lost - unless you start using lab gear.
If your freezer is cold enough, there won't be much alkaloid left in it after freeze precip. That's another reason to argue against evaporating the naphtha.

The mini A/B is a nice exercise, and quite satisfying if you like tinkering in the kitchen laboratory

 

[fidus-archimedes]

I had similar issue. I used a beer growler for my pulls. I had to leave about 50ml of naphtha behind on every pull to keep from siphoning the soup. I still got plenty of product, so it wasn't a big concern, but I do wish I'd had an Erlenmeyer at the end.