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Benefits of freeze vs evaporation? Options
 
isambard
#1 Posted : 7/14/2008 6:44:24 AM

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I'm new here and still learning the tricks of extraction. I'm in the midst of my first batch and it's going well I think. I've done loads of reading on here but there are still a couple of questions which I haven't got clarity on yet, hope you good folks can help me out?

Can someone explain whether freeze precip is better for getting DRY, naptha-free product than evapping in a pan is?? I'm evapping with a fan right now and my solvent is giving me crystals, which I've scraped and set aside. They smell a bit of solvent though. How long till they dry out completely? If they still smell a bit of solvent, does it really matter?

Does freeze evap help this drying process? If the crystals are ice cold, are they going to be cleaner? I don't quite get why freeze precip = cleaner. When you scrape out of the jar etc, the crystals are still doused in naptha and have to be dried out before smoking. Is this any different from just evapping all the naptha away as I'm doing and then harvesting the crystals? In short, do cold crystals dry more completely?

What I'm getting are mainly white, with some yellowish, crystals once the vast majority of the naptha is gone. There's a lingering odor of naptha though so I'm guessing I just need to wait it out and allow all trace of naptha to evaporate. Is that correct?

Also, as far as NaOH residues getting into the DMT and thus requiring a 'clean', which I see mentioned a lot, I'm assuming that it's not possible for NaOH to be in the naptha solution. Am I right? When you folks talk of 'cleaning', you're cleaning out fats/ oils that originate in the plant material rather than thinking about lye contamination, right? I can't see how lye could cross over into the naptha, given that the separation between the base sludge and the solvent is, as far as I can figure, absolute.

This is coming from a place where I guess I'm quickly realising I should probably be freeze precipitating, as all you experienced SWIMs seem to be doing it that way. But I'm yet to understand how the benefits of doing it that way outweigh the labour/ extra steps required. Is the spice experience much better for it?

Which raises a wider question perhaps. Does purity of spice matter much? That must sound like sacrilege! But I mean, if there's slight oil contamination/ discolouration, or your crystals aren't gleaming white shards of perfection, does it really affect the journey? From some reports, even blackened leftovers from the pipe seem to do the trick. I figure if there's DMT in it, then you're off to DMT space regardless of the aesthetic quality or a few residuals. I want someone to say: "Yes! Lazy noob! Just evap your naptha off, scrape up whatever gunk's left and smoke it! It's easy!" (For the record, quite nice fluffy white crystals rather than gunk). Unless of course I'm making some wrongheaded errors in my thinking on this - quite probably am - in which case I hope you gentle souls will set me straight.
 

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Infundibulum
#2 Posted : 7/14/2008 11:07:51 AM

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Lazy noob! Just evap your naptha off, scrape up whatever gunk's left and smoke it! It's easy!Razz

It doesn't matter which way you do it, evap or freeze-precipitate, you'll most likely get something smokable in the end.

People are not anal with purity. If your hobby is extractions then you enjoy extractions as much as the final product. It's all about the extraction enthusiasm that makes people want to extract different stuff with different procedures and different solvents, separate dmt from 5-meo-dmt, grow crystals with different shapes from different solvents etc.



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endlessness
#3 Posted : 7/14/2008 11:21:14 AM

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isambard wrote:


Can someone explain whether freeze precip is better for getting DRY, naptha-free product than evapping in a pan is?? I'm evapping with a fan right now and my solvent is giving me crystals, which I've scraped and set aside. They smell a bit of solvent though. How long till they dry out completely? If they still smell a bit of solvent, does it really matter?

Does freeze evap help this drying process? If the crystals are ice cold, are they going to be cleaner? I don't quite get why freeze precip = cleaner. When you scrape out of the jar etc, the crystals are still doused in naptha and have to be dried out before smoking. Is this any different from just evapping all the naptha away as I'm doing and then harvesting the crystals? In short, do cold crystals dry more completely?


yes freeze precipitation generally yields purer crystals. At room temperature or higher, the solvent will dissolve both the dmt, but also some other impurities. At freeze temperatures, if the solution is saturated, all the dmt will precipitate (get stuck to the bottom and side of the glass) while some of the impurities will still stay dissolved in the solvent

so when you take it out of the fridge, you quickly scrape the crystals stuck to the side (you have to do it quick, because as the temperature rises after you take it from the fridge, the dmt starts dissolving again).. When you scrape the crystals, they will start floating in the solvent, so you quickly pass this solvent through a coffee filter already attached on another container.. The DMT crystals will stay on the coffee filter, and the naphtha with some impurities will pass through..

Then you just open the coffee filter up and spread a bit the crystals. The dmt crystals will be mostly dry since the naphtha passed through the filter, but just leave it for a while to completely evaporate.. it takes only a few minutes.

if you just evaporate instead, all the impurities will stay with it (might not be so bad but if you want the purest possible product, then freeze precip is the way to go)

isambard wrote:

What I'm getting are mainly white, with some yellowish, crystals once the vast majority of the naptha is gone. There's a lingering odor of naptha though so I'm guessing I just need to wait it out and allow all trace of naptha to evaporate. Is that correct?


yes that is correct...

isambard wrote:


Also, as far as NaOH residues getting into the DMT and thus requiring a 'clean', which I see mentioned a lot, I'm assuming that it's not possible for NaOH to be in the naptha solution. Am I right? When you folks talk of 'cleaning', you're cleaning out fats/ oils that originate in the plant material rather than thinking about lye contamination, right? I can't see how lye could cross over into the naptha, given that the separation between the base sludge and the solvent is, as far as I can figure, absolute.


well yes and no. In general the NaOH is not soluble in naphtha at all, but it is possible that there are ions, traces of it, specially if you use a STB tek with high amounts of NaOH. Other ppl here can inform you better im sure. anyways SWIM definitely suggests doing a sodium carbonate wash since its easy, cheap and will guarantee a purer product.

The fats and oils are not cleaned, as far as I know, with ammonia/sodium carbonate wash. They would only be cleaned with recrystalization

isambard wrote:

This is coming from a place where I guess I'm quickly realising I should probably be freeze precipitating, as all you experienced SWIMs seem to be doing it that way. But I'm yet to understand how the benefits of doing it that way outweigh the labour/ extra steps required. Is the spice experience much better for it?


First time SWIM also thought it seemed like too much work but in the end its very easy and actually a fun part of the process..

isambard wrote:

Which raises a wider question perhaps. Does purity of spice matter much? That must sound like sacrilege! But I mean, if there's slight oil contamination/ discolouration, or your crystals aren't gleaming white shards of perfection, does it really affect the journey? From some reports, even blackened leftovers from the pipe seem to do the trick. I figure if there's DMT in it, then you're off to DMT space regardless of the aesthetic quality or a few residuals. I want someone to say: "Yes! Lazy noob! Just evap your naptha off, scrape up whatever gunk's left and smoke it! It's easy!" (For the record, quite nice fluffy white crystals rather than gunk). Unless of course I'm making some wrongheaded errors in my thinking on this - quite probably am - in which case I hope you gentle souls will set me straight.


well its many things at once. Firstly, you´re right you dont need the purest white to have a very strong experience. Secondly, there are reports that a particular type of yellowish oil, maybe dmt oxide, can be even stronger than dmt. BUT... its all about what you want and how much time and patience you have .. Personally, SWIM likes to have the purest possible product. SWIM is never in a hurry when making this anyways, and its actually very little extra work to have very pure stuff (sodium carbonate wash that takes 2 mins, freeze precip which takes same amount of time imo as evaporation, plus maybe 1 or 2 recrystalizations, which I just leave in the fridge overnight).

SWIM always feels like making sure there is no chemical remains, but also diminishing the amount of plant oils and so on. Any smoke is a bit aggressive on the lungs, so SWIM feels like achieving the purest possible product to only irritate the lungs as much as necessary (even though SWIM only smokes DMT rarely anyways, but still...)

lastly, SWIM has already taken freebase DMT orally and likes to have this possibility in his ´magic box´.. In the case of ingesting, SWIM wants to make sure that he is ingesting no chemicals at all, so having the purest DMT is always good because if wanted, it can be ingested orally too


hope that helps.. any more questions, feel free to ask
 
notapillow
#4 Posted : 7/18/2008 2:32:27 AM
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wow
that was very helpful

thank you


freeze persipe has always bafled me. but then again i only tryed it once and it was a trial run with only 50 grams of bark and far far too much naptha.
so in the end i got a huge jar of naptha with 2 little streaks of white on the side.

nothing to right home about



but im sure i could try it next time

would you mind walking me through your steps


the time constraint always worrys me
 
endlessness
#5 Posted : 7/18/2008 12:52:01 PM

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notapillow wrote:
wow
that was very helpful

thank you


freeze persipe has always bafled me. but then again i only tryed it once and it was a trial run with only 50 grams of bark and far far too much naptha.
so in the end i got a huge jar of naptha with 2 little streaks of white on the side.

nothing to right home about



but im sure i could try it next time

would you mind walking me through your steps


the time constraint always worrys me


well, the trick is to pre evaporate most of the naphta before sticking in the freezer.. If there is too much naphtha, then even at freeze temperatures, a lot of the dmt will stay dissolved in it, wont precipitate.. So what you have to do is to saturate the solution, or in other words have less naphtha per dmt, and then sticking in the fridge.. To do this, you just evaporate the naptha to a small amount, and then stick it in the fridge

so for example, SWIM makes a pull with 250ml with naphtha... Then SWIM will evap it down to less than 100ml, maybe 50ml.. If too little is pre-evapped, the solution wont be saturated enough so not all DMT will precipitate.. you dont have to worry about pre-evapping ´too much´, as nothing bad can come out of that.. The most that will happen if you pre-evap a lot, is that some crystals will start being formed even before you stick it in the freezer..

So anyways, the rest I explained in the other post.. You basicaly put it in the freezer overnight, in the morning put a coffee filter on top of a glass, then take out the container from the freezer and quickly scrape the sides and bottom, pass the liquid through the coffee filter. The DMT will stay on top of the filter while the naphtha will pass through. So open up the coffee filter and let the crystals finish drying. Maybe there will still be some crystals stuck to the side of the container which werent properly scratched, so you just scratch these left overs and put them on top of the coffee filter too...

you dont have to worry about having to be too fast in doing this, because the most that will happen is some dmt will get redissolved.. But you wont lose it, it will be there in the naphtha, so in the worse case you just stick it in the freezer again or evaporate it all if you give up on this technique

Smile
 
Spock's Brain
#6 Posted : 7/20/2008 8:34:38 PM

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I may be worng about this, but I don't get the coffee filter method. I find it advisable after pulling it out of the freeer to just pour the solvent off the crystals that are stuck to the surface of the plate. Then, just set the plate out to let the remainder evap away. I set the plate on a ice bath to keep it cold while the remaining solvent evaps away...
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KUSHMASTER
#7 Posted : 7/20/2008 9:49:23 PM

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Same here, except swim should try the ice thing. Swim just puts it at an angle to let any remaining naptha drain down into a jar. Seems to work well.



All my posts are hypothetical and for educational/entertainment purposes, and are not an endorsement of said activities. SWIM (a character based on other people) obtained a license for said activity or did said activity where it is legal to do so.
 
fourthripley
#8 Posted : 7/20/2008 10:36:51 PM
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To filter freeze precip. I take a large container with a lid that will fit in my freezer and has enough room to take a jar and funnel, pre-chill it for 15/20 minutes and then quickly pour the solvent in and just leave in freezer until done. Removes any redisolution worries although I'm not sure if it's just superstition anyway; I've had jars of solvent with freeze precip. product sitting in the bottom for a week or so- were dirty and needed heating up and 'washing'- without noticeable redissolving.
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shoe
#9 Posted : 7/20/2008 11:47:21 PM

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Just for the record, I don't agree with filtering freeze percipitates with coffee iflters. due to the waxy nature of DMt you will just loose it all into the paper.

Freeze percip, and then decant carefully, while still freezing, and then just evap the crystals till dry.

Btw: the purity of the crystals is nothing to do with how much naptha is left on them. we're talking about tan wax < orange/yellow wax < yellow shards < yellow powder < white powder < clear crystal
shoe

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shoe
#10 Posted : 7/20/2008 11:49:04 PM

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Spock's Brain wrote:
I set the plate on a ice bath to keep it cold while the remaining solvent evaps away...


whats the point, you've allready poured off the grease? it doesnt matter if they re-dissolve because they're only gonna come out again. if anything its advisable to heat them at this point, to speed evaporation of the tiny bit of remaining naptha.
shoe

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endlessness
#11 Posted : 7/21/2008 5:23:25 PM

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SWIM tried both these ways...

When pouring the naphtha off, the crystals in the side of the glass started melting down due to the small amount of naphtha that was trapped between the crystals and warmed up.. So then SWIM´s crystals melted off into a goo that resisted crystallizing... So if you guys decide to go this way, then I would suggest tilting the container so that remaining naphtha drops away instead of collecting inside it, and also maybe putting a fan to accelerate the process


with the coffee filter for SWIM it has been working perfectly... maybe a few factors are involved why it works for some are not for others:

- the type of coffee filter (maybe too porous would absorb dmt)

- how fast the naphtha is filtered (if it takes too long, the dmt might melt and get absorbed in the paper)

-size of crystals (too small might melt too fast)



 
isambard
#12 Posted : 7/22/2008 9:50:50 AM

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Thanks for all responses .. plenty to ponder. I've been on holiday for a week, returning back to a stack of crystals that have lost all trace of the naptha. I'll see how I get on with these, but in future (I have a final extraction to do, then a batch of MHRB waiting to be processed) I will go with the freeze precip .. sounds good and clean.

Peace earthlings.
 
 
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