Freeze precip help?

[SHroomtroll]

I have some problems with the steps after i pulled out the naphta from the lye.

I pour the naptha in glass jars and put them in the freezer, a day later i have some crystals in the bottom.

But when i pour out the naphta for evap alot sticks to the bottom of the jar, i have tried to scrape it off with a knife of something but it´s preety stuck.

I´m thinking about putting some naptha back in the jar and then warm it a bit in warm water and then try to scrape and shake up the crystals to pour our.

would this work or does anyone else have another idea?

 

[endlessness]

you can either try to find a better tool for scraping the crystals, or for next time you can find a container shaped in a way which allows better access to scrape the crystals. As for now, yeah you can use a small amount of warm naphtha to redissolve the crystals and evaporate it (or freeze in a better container), or you can use some ethanol/ipa/acetone to also pick up and re-evap somewhere else.

 

[rave420]

instead of finding a better tool for "scraping" find a better container for recrystallization

i found small plastic ziploc containers to work SO MUCH BETTER! the crystals still stick to the side, but they only take one gentle nudge and they fall right off the plastic. Even just swirling the cold naphtha around loosens all the crystals.

I don't know why people are so stuck on recrystallizing in glass. DMT freebase bonds quite good with glass surfaces. Not so with plastic. Sure, if you got a more aggressive solvent, but naphtha + plastic + freezer = lotsa crystals and a spotless dish.

So run hot naphtha through your dish to get all that's stuck on, and recrystallize in a plastic container. It will NOT stick, i guarantee

 

[endlessness]

what plastic is ziplock container made of? I wouldnt use that unless I was absolutely sure there was no problem with naphtha + that particular plastic

 

[rave420]

Plastic Ziploc containers are perfectly safe to use with naphtha. I have used the same container for some 20+ recrystalizations, and the solvent leaves the plastic alone. It's the same plastic the plastic my eyedropper and turkey baster is made from.

Don't use the plastic dish with any other solvent than naphtha though, for obvious reasons.
They are made from Polypropylene and do not seem to be attacked or degraded by ice cold naphtha.

 

[SHroomtroll]

Ok i will try using that the next time, i have expermented a few days now trying to get the precioius out of the naphta but no real yields yet, i only made a extraction with 80grams but still ive only pulled out about 100miligrams so far.

But now i have put in a little more lye in the jars and tried to heat it a bit too, also i reevaluated my freeze precip tek and came up with this.


1. Pour the naphta out from the lye/mimosa mix, into 2 jars that go in the fridge,

2. after 24hours i take the jars out and carefully pour the naphta through some coffe filters to a oven dish. trying to leave as much crystals in the bottom of the jars left.

3. i put the dish with the filtered naphta back in the freezer to freeze out any last crystals.

4. i use warm acetone to wash the crystals off the coofe filters and the empty jars and pour all the acetone in another oven dish for evap.

5. i take out first dish that´s been in the freezer for a few hours and formed new crystals, i pour this naphta back in the jars with lye/mimosa and then wash the oven dish with acetone to get all the crystals of then in the other dish with acetone.


This way i don´t need to evap any nasty naphta in my appartment and can instead only evap acetone which is much faster.




I´m waiting for my first batch using this tech and so far it looks alot better than the minimal spread out yields i got when trying to evap naphta.



Edit: another advantage i think is that since acetone evaps alot faster than naphta, the crystals will probably oxidate alot less sincew they don´t have to be in contact with air as much.

 

[Trickster]

... ive only pulled out about 100miligrams so far.

You should aim at 0.5 g at least.

1. Pour the naphta out from the lye/mimosa mix, into 2 jars that go in the fridge,

I suggest to do at least 3 naphta pulls.

Unless your pulls are very different, i.e. one is substantially dirtier than others there is no point in processing them separately. Usually I combine all pulls together.

It is adviseable to reduce your pulls until you have saturated solution. Otherwise lots of goodies will remain in naphta. I reduce my combined pulls to at least 1/5th of the original volume.

To minimize your losses, either you reduce your naphta before freeze-precip, or you will have to evaporate the remaining naphta after the freeze-precip.

2. after 24hours i take the jars out and carefully pour the naphta through some coffe filters to a oven dish. trying to leave as much crystals in the bottom of the jars left.

Usually the spice is stuck to the beaker walls in clumps. IME there are very few free-floating crystals. They are more dense than naphta and fall to the bottom. Careful decanting is all you need. Leave a few last naphta drops in the beaker to be on the safe side. Filtering = hassle + losses.

3. i put the dish with the filtered naphta back in the freezer to freeze out any last crystals.

That is pretty much useless. You may get some more goodies from that naphta, but only if you reduce it substantially.

This way i don´t need to evap any nasty naphta in my appartment and can instead only evap acetone which is much faster.

I do not think acetone is much better to evaporate in an apartment. A more radical solution would be to assemble a home-made distillation apparatus. You will find it useful quite often. E.g. you may run your inexpensive technical grade solvents through it and make them much cleaner. A vacuum distillation setup would be even better. I've assembled mine for less than $100.

... the crystals will probably oxidate alot less sincew they don´t have to be in contact with air as much.

IME it is not an issue.

 

[DoingKermit]

I think you are making the process more complicated than it needs to be. Make sure you pool all your pulls together in a small jar/glass dish and evaporate it down to about 1/10th of the original volume. This makes a very saturated solution which will allow most of the dmt to stick to the glass and not float around in your cold naphtha.

After about 24 hours, you can pour the cold naphtha back into the mimosa/lye mix (to catch anything missed next time round), leaving all crystals stuck to glass behind. If using a jar, you can screw the lid back on and shuv jar back into freezer upside-down. This allows remaining solvent to drip out into lid. After a couple hours, remove jar from freezer (kept upside down) and unscrew cap making sure to leave remaining solvent in the lid.

Now place your jar with DMT under a fan to evap the remaining solvent. Tadaaaaaaah! No need to worry about filters and multiple freezing. Good luck to ya

 

[soulfood]

There's a much simpler option than all of this.

Rather than putting your solvent straight to the freezer causing fast precipitation, place it in the fridge and over time watch the solution go cloudy and actually shards will start to form. Then when the solution clears, place it in the freezer to finish off the precip/formation. These crystals are much more sturdy and easier to handle and all it really takes is 12 hours in the fridge then 12 hours in the freezer. As they form more slowly, they shall also be more pure with no need to recrystalise around 90% of the time.

 

[DoingKermit]

So true, soulfood. I have done that too with great results. Instead of scraping off crystals you just need to flick them off with a knife or something similar.

 

[SHroomtroll]

Ok thanks guys i got alot of new ideas from this...

Evaping naphta seems like a dead end for me since it stinks way to much and takes to long, even if i let the dish stand out for an entire day it won´t evap to much and leaves a very heavy cloud of stinky in my whole apartment, acetone on the other hand i can leave 200ml out over the night and it will be gone the day after.


HOnestly i have done like 3pulls already and the first 2 i just reused the naphta since i dint get almost anything out, this was probably from problems with the lye/mimosa goo than the naphta pulls itself.


Today i scraped up the first real pull where i used the method i wrote down, i would estimateabout 0,1-0,2 in mixed colour crystals and it smells really nice


i have now done a second pull that way and washed all the dishes and filters i used with acetone and put it all in a dish... on the first look of things it seems to be alot more than the first pull so i´m hoping for a 0,5 total after this one.



Tomorow when i do my next pull i will try this then...

1. pour out all the naphta from the mix and put it in the window behind curtains with a room temp fan over it,

2. afterevaping it i will put it all in one jar that goes in the fridge 12hours? then in the freezer 12more hours?

3. carefully decant all the naphta (through a filter why not)

4. scrape/acetone wash my jar and filters and put in a dish to evap.

5. scrape of all the goodies from the dish then splash the dish with some acetone and put some weed or tobacco in it and try to scrape of any leftovers.

6. reuse naphta a few more times to make sure i don´t throw anything away.

 

[Trickster]

Ok thanks guys i got alot of new ideas from this...

Evaping naphta seems like a dead end for me since it stinks way to much and takes to long, even if i let the dish stand out for an entire day it won´t evap to much and leaves a very heavy cloud of stinky in my whole apartment,

In the past I did it quite a few times in an apartment. I have evaporated 200 ml of naphta in less than 2 hours. Things that GREATLY increase evaporation speed:

1. Use evaporation container as wide as possible.
2. Create a fast airflow over the solvent surface. A fan or a hair dryer works fine.
3. Heat the solvent. Remember, no open flame!

If you do that on a rainy night there is very little chance anybody notice.

 

[Trickster]

HOnestly i have done like 3pulls already and the first 2 i just reused the naphta since i dint get almost anything out, this was probably from problems with the lye/mimosa goo than the naphta pulls itself.

No, most probably this is because your naphta pulls were not saturated enough. If your naphta is very far from being saturated, cooling it may not make it saturated, so, no spice will precipitate.

 

[SHroomtroll]

Ok nice, that explains why i didnt get anything out before, i admit that recent attempts of evaping naphta consisted off leaving oven dishes full of the stuff over night with not to much effect,

now i have put it in front of a 2kw heat fan, although i keep it on low heat to not risc any accidents,

I think there should be a sticky about npahta evoparration/freeze precipition since this seems to be the hardest part off the the tek.

 

[SHroomtroll]

Now we are talking extraction :d

Have about 05-07 of nice crystals i just made to changa, will blast off in a few hours, thanks guys :shock:

 

[Trickster]

... will blast off in a few hours, thanks guys :shock:

Safe journey!