Water/heptane Recrystallization method?

[NullEntity]

From what i know most Recrystallization tek's dissolve spice in N-heptane via hot water bath and decanting leaving heavy impurities at the bottom. then slowly cooling etc.

i was wondering, as heptane is non-polar and is lighter in density compared to water, is it possible to add water to a already heptane dissolved solution with spice in it already and in theory all the lye and garbage sink below the heptane and into the water allowing for easier decanting of heptane, get lower loss and not worry about picking up the sentiments/lye at the bottom ?

i have seen naphtha after decanting from basified solution being washed into water then decanted from the water but i haven't seen the concept being used for recrystallization with heptane. is it a specific reason, or is it just hasn't bin done yet ?!

i want a godly pure end result and loss of yield is the price to pay i understand that but the thought of the possibility making the process better keeps me up at night. There is a beautiful amount of extraction teks, but the methods for purifying are lacking in comparison, in my opinion. does any one know more on this ?

 

[HippyDippy]

SWIM did this very thing last night. There was leftovers after doing a previous decant and recrystallization, and SWIM wondered if they could get anymore spice from the goo leftovers.
SWIM added the heptane wash to about 100ml of straight water and shook it 4-5 times about 5 min apart. Once the heptane was removed from the water, it was sent to the fridge and then the freezer to precipitate. No crystals as of this morning. If there are still none forming by 5pm the solution will be evaporated by half, and freeze precipitation will be tried again.



You can see how all the crap floating in the heptane from the first picture is captured in the water in the second pic.
Hope this helps

 

[NullEntity]

This is very helpful information, but i was talking about in the sense of using it in the process of recrystallization of spice not to extract spice from left over sentiment from a previous Recrystallization. regardless the info is still useful hopefully SWIM can obtain trace amounts of spice from the sentiments as well that would also be amazing.

 

[Jees]

From what i know most Recrystallization tek's dissolve spice in N-heptane via hot water bath and decanting leaving heavy impurities at the bottom...

...i want a godly pure end result and loss of yield is the price to pay i understand that but the thought of the possibility making the process better keeps me up at night. There is a beautiful amount of extraction teks, but the methods for purifying are lacking in comparison, in my opinion. does any one know more on this ?

Hi NullEntity,

The whites are not really better than the yellows or the oils, really. All is dmt just another jacket. Get rid of the caustic, water wash if you feel so, very good, from then on you get very high quality deems.

Allow me to re-quote myself from an earlier post:

...Hopefully you're aware the goo is not to throw away, some people think it's impurities to discard, there is a hoax out there, it's very much very active dmt in oily form. If you're sure all caustic was out, it's blazingly usable...

Fancy white is cool candy looking, and there are some threads here to re-form oil to white texture, there is some progress but not really a golden bullet ideal workflow that nails it 100% each time, it's ongoing.

I bet water washing a spice loaded naphtha pull, or water washing a spice loaded re-x heptane, makes no difference. Only, Re-x is such a small volume that water washing that might affect separation of layers, but I havent tried that. If you're keen on water washing, why not the naphtha pull? You would grab any residual caustic there, and omit fuzzing with the small volume re-x heptane.

Happy trials...

 

[downwardsfromzero]

SWIM? So noughties. No need to swim here.
Most of the dark oily stuff that collects at the bottom of a heptane re-x is DMT oligomers - that is, assuming you've separated your naphtha sufficiently carefully and competently from the base soup. The way to deal with oligomers is via a mini-A/B process.

IME, observing heptane solution of freebase over a longer period shows that the amount of oligomer increases, as does the degree of oligomerisation - the oily goo gets darker. Water washing would clear up base contamination but you shouldn't have let that get into the freebase crystals in the first place. Let your pulls settle in a Pyrex jug before transferring them into the freeze precip dish and you should get clean crystals 99% of the time.

You could wash the naphtha pulls with something like saturated brine or washing soda solution but it's preferable to work meticulously rather than adding an extra step where further losses or mistakes could occur.

 

[Toshido]

SWIM? So noughties. No need to swim here.

Yeah, using SWIM doesn't absolve you from legal troubles, so don't waste your time with it.

Let your pulls settle in a Pyrex jug before transferring them into the freeze precip dish and you should get clean crystals 99% of the time.

This. When I pull, I transfer to a 500mL beaker. When the solvent cools, the impurities will drop to the bottom first, allowing you to decant the dmt containing solvent while leaving behind said impurities.

If you pull straight to a dish, you run the risk of accidentally sucking up some soup and transferring it to the dish. Having a vessel in between your pulls and crystallization dish help to mitigate that.

Now, I pull directly into a separatory funnel and then do a sodium carbonate wash, but even then it's tricky, the sep funnel can be dangerous, and I still get a tiny bit of goo sometimes after a wash because of how the valve system can trap tiny droplets of goo. It's hard to spot!

 

[HippyDippy]

Yeah, using SWIM doesn't absolve you from legal troubles, so don't waste your time with it.

Ok fair enough. Being a new user I was trying to follow the lead of other users.

This is very helpful information, but i was talking about in the sense of using it in the process of recrystallization of spice not to extract spice from left over sentiment from a previous Recrystallization. regardless the info is still useful hopefully SWIM can obtain trace amounts of spice from the sentiments as well that would also be amazing.

NullEntity, I was just trying to be helpful by letting you know that you could in fact combine water with heptane just like you can with water and naptha. The water does not mix with the NPS, which is where the DMT is held, but the water does combine with other stuff.

This is still only my first run, so I am learning as I go. I had the same question as you did. With over 1.8 million posts on this forum, research can only get you so far in a short time. It can be far quicker to just ask the question in a new post.


Results from the re-x: The jar is currently in the freezer. Yesterday when I got home from work, no crystals had been formed. So, I reduced the liquid by over half by evaporation, and put it back in the freezer. This morning, we have growth!!!!

seiten zum uploaden

 

[fractals4life]

I pull into a measuring cylinder already (exactly) half full with distilled water, making sure to give the NPS a good squirt into the cylinder so it goes well down into the water and splits into tiny droplets before settling out.

That way I get a water wash of my NPS and easy knowledge of how much NPS got left behind per pull.

It's also easy to pipette the NPS off the top of the water due to the long thin measuring cylinder.

Cheers,
frac4