solvent evaporation

[chezzy]

Current procedure is a straight to base using NaOH then a naptha pull on powdered MHRB.

First question, what are my options ( and consequences ) to speed up evaporation of solvent?

Second - is there any benefit from setting up glassware to keep this solvent rather than lose it to air or would it contain impurities that prevent it's reuse?

Third - what aspects contribute to crystal size? If I wanted larger, prettier crystals, what should I be aiming to improve?

Thanks

 

[vibrancy3]

1. Welll i have heard doing a part room temp evapouration, then freeze precipitation is not only faster but provides more xtals in your yeild

(so that would maybe be 1:1 ratio of 12hours room temp evap and 12 hours freeze precip)

2. I dont quite understand the nature of this question but i do keep my used naphtha in a glass for future extractions

(say i am doing an extraction 40g of mhrb i will use 50ml of new naphtha for first pull. then use 35ml of used naphta for 2nd pull and 25ml o used naphtha for 3rd pull)

3. for more larger, prettyier (lol) xtals i would say more time freeze preciping, swirl/roll your solution for a longer period of time (avoiding emulsions of course)

you should look on the FAQ for more better info

 

[chezzy]

now I'm really confused!

I've got maybe 200ml of naptha in a pyrex dish by an open window evaporating into the air. How am I meant to save any of this? My intent was to leave it to evaporate until there was just DMT crystal left - am I missing something important?

What options are there for getting crystals out and not losing solvent? I'd presumed that either I lose it to the air, or I set up glassware capture it from the system. Please help, I know you guys get asked questions every day but FAQ's etc aren't always helpful if you're not used to this specific forum's lingo and culture.

Thanks.

 

[Elf Machine]

Since you can't precipitate out your freebase DMT out of naptha via titration or gas bubbling, it only leaves distillation or freeze precip. Throw it in the freezer for a couple days.

 

[chezzy]

I thought the DMT is mhrb is not freebase but a salt form?

In the past I've let the solvent evaporate to form crystal no problem at all. Would be nice to improve on the method and get more understanding if someone can help please.

Thanks.

 

[Elf Machine]

Compounds need not be salts to precipitate out in crystaline structure. In fact, many if not most solids do this. The DMT in MHRB I believe is in salt form but the acid it's bonded to is knocked off by the base you add leaving you with freebase DMT which you take up with the non-polar.

 

[gammagore]

The tek you are using gives you freebase.

Evaping it all the way takes long and gives a dirtier molecule. Not to mention wastes alot of solvent.
Better to evap it till it gets cloudy when you blow on it(super saturated), then freeze precip it, collect xtals and save the naptha.

No need for any glassware setup, just store it in a glass bottle.

To grow big xtals, after the DMT from the freeze precip has been collected, disolve this dmt in a small amount of clean naptha/heptane, say 50ml/gr DMT. Leave it in a small glass/wine glass with a coaster covering it, leaving just a small space for airflow. Leave this somwhere undisturbed for a week or so.

Freeze precip that naptha

 

[GalactivatedMuse]

any way to evap faster?

 

[Electric.Sight]

^^^^^^^
Using a fan at room temperature can speed up evaporation. Using a hot fan may lead to oxidization and a gooey product.
The fan should probably be removed when the amount of solvent left is low, and just let the rest naturally evaporate.

 

[chezzy]

thanks everyone, very helpful. Last questions for this thread...

So my bowl now has a cloudy liquid (naptha + freebase DMT). This is going into a jamjar then into the freezer for 24 hours or so.

Questions 1: there are crystals all over the sides where it's evaporated and the bottom of the bowl. Pure white. Should I save these, are they freebase DMT?

Question 2: please confirm my understanding is correct: the NaOH deprotonises the DMT salt, which makes it freebase - this is non polar, and so is soluble in the non-polar solvent. Freezing the solvent lowers it's ability is hold solute so it crashes out of solution. Is this correct?

Question 3: What's the best way to get the DMT crystals out of liquid (and cold) naptha? Will a fluted coffee filter do? I've only ever evaporated dry before.

Thanks guys, and thanks for the help this far, I already have a better undersatnding of what I'm doing I think.

 

[Elf Machine]

#1 Yes

#2 Yes

#3 Best way is vacuum through buchner. Never used coffee filter but should work.

 

[chezzy]

#1 Yes

#2 Yes

#3 Best way is vacuum through buchner. Never used coffee filter but should work.

thanks Elf Machine. Great help here and above mate.

Right, digging out my lab notes to look it up rather than clog the forum.

There's actually a load of crystal in the bowl now solvent has been poured off, maybe 1g-ish.

Would you add a salt or leave it as freebase?

 

[gammagore]

That freebase is the end product, make sure its dry and solvent free and vape it

No need for adding any salt to that.

 

[SHroomtroll]

Most of the visible crystals seems to stick to the bottom of my jars, could it work to heat the jar with a bit of naptha in to melt the crystals and then pour the naphta with the crystals out?