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How greatly is yield effected by evaporation prior to freeze precipitating Options
 
Al-Wasi
#1 Posted : 11/24/2018 6:13:00 PM

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Post subject basically says it all. Been extracting dmt for around 5 years and I've never done the recommended evaporation of half of the NPS prior to freeze precipitating. Wondering how greatly is my yield affected by this ie is there a bunch of dmt left in the NPS that won't crash out ?

I guess another question I have while I'm at it is in regards to just totally evaporating the NPS rather then freezing altogether. When doing this is the final product the same as from freezing or is it more oily waxy etc?
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Jagube
#2 Posted : 11/24/2018 6:26:06 PM

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I don't think it affects the total yield that much, only the yield from each pull. And when each pull yields less, you'll still get most of the goodies out, it just takes more pulls.
 
Al-Wasi
#3 Posted : 11/24/2018 6:30:10 PM

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Pretty sure it's stated somewhere here that dmt has a hard time crashing out of solutions that aren't all that saturated . I've always took that to mean that once alot crashes out and the NPS becomes less saturated it stops to crash out although the NPS still contains dmt. There fore you can evaporate some to get the concentration higher again and more will then crash out .

Is this logic correct

Edit
Quote:
The amount that one should pre-evaporate depends of course on how much solvent used. The idea about pre-evap is that the solvent should be as saturated as possible with dmt so that most or all of it precipitates when put in the freezer. If its not saturated enough, then not much (or not at all) will precipitate. So if one used more than 3:1 ratio of bark:solvent, then pre-evaporate enough to reach the equivalent of it (so if one used, lets say, 100ml per 100g bark, pre evaporating till a third of original volume is recommended). Here's an attempt to explain why not having it saturated enough may result in no or low yield


Later pulls will most likely be less saturated with dmt than first pulls, so for the later pulls (like lets say the 4th and 5th), it would be logical to pre-evaporate even more than the first pulls. In the example given above, instead of evaporating until a third of original volume, maybe one could evaporate until there is only a quarter or a fifth of original volume.

Some people gauge the amount of pre-evaporation by doing it until the solvent starts getting cloudy.

In any case, remember to re-use the naphtha after retrieving the crystals from precipitation, and/or evaporating it all the way down to see if there are any actives that remained in the naphtha after the freeze precipitation
from the faq
That moment when you wonder if this time you went too far....

Obviously everything discussed here is the fictional accounts of someone with an out there imagination. I mean really could any of these tales be real?
 
Nydex
#4 Posted : 11/24/2018 6:51:08 PM

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Interesting, I'd love to hear other people's findings.

On my first and only spice extraction I've done so far I just put the dish straight into the freezer without pre-evap and got around 1g of yellowy crystals from around 40g of MHRB, which is supposed to be quite a good yield according to the people I've discussed it with.

I used cyb's hybrid atb salt tek. Soon I shall do a second go at it, this time with the max ion tek and ACRB.

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Trickster
#5 Posted : 11/24/2018 7:44:35 PM

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Pre-evap is necessary to make the NPS solution saturated to the point when DMT starts to crash out.

Freezing NPS solution makes most, but not all, DMT to crash out. A small amount of DMT always remains in the NPS even a low temperatures. So the the smaller the NPS volume the better your yield. To check it you may you evaporate the NPS decanted from freeze-precipitated DMT. There always be some small amount of DMT remaining.

So, why then we freeze-precipitate DMT instead of evapping the NPS completely? This is because NPS also dissolves some impurities that do not crash out even at low temperatures. It allows to obtain more pure product. If the NPS volume is small DMT losses will be negligible.

How to know when to stop reducing the NPS solution? When your NPS gets cloudy close to its boiling point you may stop reducing it.

It is also advisable to use NPS with high DMT solubility at boiling temp and low solubility at low temp e.g. heptane.

To obtain pure crystalline DMT several re-crystallizations may be required.

Usually I evap combined NPS pulls completely and obtain honey-colored thick oil. Then I extract it 5-7 times with small amounts of Heptane (10-20ml), combine these pulls and reduce the volume until Heptane becomes milky-white, keep it at RT for an hour, put it in a fridge (wrapped with a film) for another hour and then in a freezer for 8-12 hours.
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pete666
#6 Posted : 11/24/2018 8:07:18 PM

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Another reason for freeze-precip is the lye contained within the non-polar solvent (or rather within the water mixed with the solvent). With evaporation it stays within the result, but when freeze-precipitating, much of it stays in the solution and do not crash out.
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