Freeze Precipitation:Unresolved Concerns

[Portals2Eternity]

So I've decided upon June 30th or July 1st for my 1st extraction. These forums have been an invaluable resource for me, so after much, much research I feel fairly confident in my process. One thing still eludes me:

When freeze precipitating, I am preparing for having to, if necessary, use a funnel (is platic ok? I'd think no, but that's all I've got) and coffee filter. That said, I would like to simply pour off/siphon the naptha from my beaker, then tip it over (in freezer or not?) to remove all traces before drying and obtaining the spice. My concern lies in if all the spice doesn't stick to the beaker, is this really the best way? Is there anything I can do to increase the likelihood of the product sticking to glass? And how ez is it, if some is floating, to pour off/siphon off the naphtha w/o pulling up some dmt?

Also, if I first siphon or dump off the naphtha, my beaker doesn't have a lid (I'm using heavy duty baggy + tie for airtight seal) so how would I turn the beaker upside down in freezer to remove traces of naphtha? Or is this not necessary, and I could just turn upside down outside of freezer on coffee filter and/or bowl? Obviously my concern would be my product melting at room temp.

This is the final leg of my preperation, so any help is greatly appreciated. I've taken care to examine dozens of threads, and these were my remaining concerns.

 

[endlessness]

Regarding plastic, depends what kind and all but generally it's NOT recommended to use plastic with solvents for reasons written here and in the two links therein:

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

In any case if you have properly saturated your solvent and freeze precipitation worked well and you are considering discarding your solvent after filtering it when retrieving crystals, then it shouldnt matter much because even if some plasticizers dissolve in your solvent, it will be discarded. But if you are thinking of reusing the solvent, then better get a glass funnel. If you have no glass funnel and no way of buying one, maybe you can somehow attach your coffee filter to a glass container so that it doesn't fall, and that way you avoid plastic.

Regarding the freeze method, check this out: FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

The turning upside down is not strictly necessary in some cases but it can help avoid melting crystal problems in some cases.. You could just have it upside down in a plate, though better not have food in your freezer because it might have naphtha smell if you dont have it in a closed container.

As for DMT sticking to the container, I've had mixed experiences, but generally it sticks well specially if you leave it for long enough (a day or so) without moving, and your freezer is properly cold.

good luck

 

[Portals2Eternity]

Regarding plastic, depends what kind and all but generally it's NOT recommended to use plastic with solvents for reasons written here and in the two links therein:

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

In any case if you have properly saturated your solvent and freeze precipitation worked well and you are considering discarding your solvent after filtering it when retrieving crystals, then it shouldnt matter much because even if some plasticizers dissolve in your solvent, it will be discarded. But if you are thinking of reusing the solvent, then better get a glass funnel. If you have no glass funnel and no way of buying one, maybe you can somehow attach your coffee filter to a glass container so that it doesn't fall, and that way you avoid plastic.

Regarding the freeze method, check this out: FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

The turning upside down is not strictly necessary in some cases but it can help avoid melting crystal problems in some cases.. You could just have it upside down in a plate, though better not have food in your freezer because it might have naphtha smell if you dont have it in a closed container.

As for DMT sticking to the container, I've had mixed experiences, but generally it sticks well specially if you leave it for long enough (a day or so) without moving, and your freezer is properly cold.

good luck

Ty for the response! With regard to the plastic, they were EXTREMELY cheap. But I looked on them and a '2' is written on them, so I'm thinking that signifies HDPE? Like I said, I don't really wanna go that route, but will if conditions necessitate it.

I did want to save all my naphtha, to either evap down and re freeze precipitate or evaporate fully. Hypothetically, say I filter the naphtha into a mason jar, IYE should the filter be pulled tight or have some slight give?

So short of me changing my freeze precipitation container from a beaker to a mason jar (or the like) with a lid, would turning it over outside the freezer after pouring off the naphtha risk melting the dmt? If it did melt turned upside down, how would I recover the melted product (sorry if stupid question, I just wanna visualize everything that could potentially go wrong and its solution)?

In your experience when it hasn't stuck to the side, did u just filter it? Or carefully siphon? How long do I realistically have before it starts melting?
& finally *if I decide upon pouring off naphtha then putting upside down in freezer but all crystals aren't stuck, what are the ways to recover any that fall?

Thanks in advance. All help is GREATLY appreciated... Will post pics of my end result, at minimum.

 

[Portals2Eternity]

Anyone have anything to offer re: my last post? I guess my primary concern is that I don't want to use a coffee filter if not absolutely necessary, but am scared that all xtals won't stick. I plan on minimizing this problem by using 30 to 40ml of naphtha for my 50g bark, leaving it in freezer for at least 24hrs, and placing bags of ice all aroumd container. I plan to use turkey baster to suck up naphtha then pour out remaining, then put lid on and put back in freezer upside down. Bu if xtals don't stick, this process is complicated exponentially in my mind. Any solution for this? And after taking out of freezer, leave lid on until room temp, then sit in front on open window? Will fan blowing at slice oxidize it?

Sorry for the follw up questions on my own post. Ive seen so many ppl have issues with freeze precip, I'm psyching myself out trying to problem-solve pre-extraction.

 

[melotikaci]

Anyone have anything to offer re: my last post? I guess my primary concern is that I don't want to use a coffee filter if not absolutely necessary, but am scared that all xtals won't stick. I plan on minimizing this problem by using 30 to 40ml of naphtha for my 50g bark, leaving it in freezer for at least 24hrs, and placing bags of ice all aroumd container. I plan to use turkey baster to suck up naphtha then pour out remaining, then put lid on and put back in freezer upside down. Bu if xtals don't stick, this process is complicated exponentially in my mind. Any solution for this? And after taking out of freezer, leave lid on until room temp, then sit in front on open window? Will fan blowing at slice oxidize it?

Sorry for the follw up questions on my own post. Ive seen so many ppl have issues with freeze precip, I'm psyching myself out trying to problem-solve pre-extraction.

If you use syringe or big pipette to remove naphtha completely from the dish, crystals won't go anywhere and will stick to glass surface. then you can put it back into the freezer or fridge upside down.

But you should do it fast(~ <5 min, perfectly doable without a fuss) or crystals will dissolve back into the solvent.

 

[Portals2Eternity]

Anyone have anything to offer re: my last post? I guess my primary concern is that I don't want to use a coffee filter if not absolutely necessary, but am scared that all xtals won't stick. I plan on minimizing this problem by using 30 to 40ml of naphtha for my 50g bark, leaving it in freezer for at least 24hrs, and placing bags of ice all aroumd container. I plan to use turkey baster to suck up naphtha then pour out remaining, then put lid on and put back in freezer upside down. Bu if xtals don't stick, this process is complicated exponentially in my mind. Any solution for this? And after taking out of freezer, leave lid on until room temp, then sit in front on open window? Will fan blowing at slice oxidize it?

Sorry for the follw up questions on my own post. Ive seen so many ppl have issues with freeze precip, I'm psyching myself out trying to problem-solve pre-extraction.

If you use syringe or big pipette to remove naphtha completely from the dish, crystals won't go anywhere and will stick to glass surface. then you can put it back into the freezer or fridge upside down.

But you should do it fast(~ <5 min, perfectly doable without a fuss) or crystals will dissolve back into the solvent.

Oh really? So removing the naphtha via pipette completely (or as close to completely as possible) will cause the crystals to stick to the glass? I wasn't aware that'd happen, but that's amazing if so! (IYE whats the better container fore freeze precip, small square pyrex dish or half pint mason jar?)

And from doing research, I was under the impression that I had to rush pulling the naphtha post freeze, only having something like 1-2mins before xtals began dissolving...but your window of <5mins is also a great relief if true.

Thank you for the response, I could not possibly do this without you and all others at the nexus!

 

[melotikaci]

Oh really? So removing the naphtha via pipette completely (or as close to completely as possible) will cause the crystals to stick to the glass? I wasn't aware that'd happen, but that's amazing if so! (IYE whats the better container fore freeze precip, small square pyrex dish or half pint mason jar?)

And from doing research, I was under the impression that I had to rush pulling the naphtha post freeze, only having something like 1-2mins before xtals began dissolving...but your window of <5mins is also a great relief if true.

Thank you for the response, I could not possibly do this without you and all others at the nexus!

Well, as long as there is no more liquid left in the dish the crystals won't have anywhere to go or float so will stick to the surface of the glass. But anyway, be careful.

For the dish choice I prefer the ones that's easier to scrape off the crystals from. So the wider and shorter it is the better.

Removing naphtha from the dish with 10-20ml syringe or pipette takes ~1-3 minutes max and from my experience crystals should be fine during this time.

Keep in mind that naphtha reacts with plastic syringe surface and after 2-3 pulls it may become impossible to pull more naphtha with the same syringe unless you wash/clean it. So if you decide to use syringe for pulls have few of them ready. For that reason glass pipette is more convenient and faster "weapon" of choice.

 

[Portals2Eternity]

Oh really? So removing the naphtha via pipette completely (or as close to completely as possible) will cause the crystals to stick to the glass? I wasn't aware that'd happen, but that's amazing if so! (IYE whats the better container fore freeze precip, small square pyrex dish or half pint mason jar?)

And from doing research, I was under the impression that I had to rush pulling the naphtha post freeze, only having something like 1-2mins before xtals began dissolving...but your window of <5mins is also a great relief if true.

Thank you for the response, I could not possibly do this without you and all others at the nexus!

Well, as long as there is no more liquid left in the dish the crystals won't have anywhere to go or float so will stick to the surface of the glass. But anyway, be careful.

For the dish choice I prefer the ones that's easier to scrape off the crystals from. So the wider and shorter it is the better.

Removing naphtha from the dish with 10-20ml syringe or pipette takes ~1-3 minutes max and from my experience crystals should be fine during this time.

Keep in mind that naphtha reacts with plastic syringe surface and after 2-3 pulls it may become impossible to pull more naphtha with the same syringe unless you wash/clean it. So if you decide to use syringe for pulls have few of them ready. For that reason glass pipette is more convenient and faster "weapon" of choice.

At this point in time, I only have baster/pipette, so I was going to use baster, then pipette for last bit, if necessary. I'm only using glass, so plastic issues won't arise.

Tell me if I'm off-base here: if I siphon naphtha off with pipette and then transfer dish back into freezer upside down, if there are floaters that don't stick, it seems those would be lost. What if when I take out of freezer, I pour off naptha with hopefully a very low amount of floaters into the naptha I plan to save, thus not actually losing them?

I just wish there were an easy way around this problem, aside from using filter...

 

[melotikaci]

At this point in time, I only have baster/pipette, so I was going to use baster, then pipette for last bit, if necessary. I'm only using glass, so plastic issues won't arise.

Tell me if I'm off-base here: if I siphon naphtha off with pipette and then transfer dish back into freezer upside down, if there are floaters that don't stick, it seems those would be lost. What if when I take out of freezer, I pour off naptha with hopefully a very low amount of floaters into the naptha I plan to save, thus not actually losing them?

I just wish there were an easy way around this problem, aside from using filter...

I thought baster was also called pipette, I just googled it. Baster is cool.

You are missing the point that if there is no naphtha in the dish then there are no floaters. Floaters float because there is liquid in the dish, if you remove the liquid completely how and where would they float?

 

[Portals2Eternity]

At this point in time, I only have baster/pipette, so I was going to use baster, then pipette for last bit, if necessary. I'm only using glass, so plastic issues won't arise.

Tell me if I'm off-base here: if I siphon naphtha off with pipette and then transfer dish back into freezer upside down, if there are floaters that don't stick, it seems those would be lost. What if when I take out of freezer, I pour off naptha with hopefully a very low amount of floaters into the naptha I plan to save, thus not actually losing them?

I just wish there were an easy way around this problem, aside from using filter...

I thought baster was also called pipette, I just googled it. Baster is cool.

You are missing the point that if there is no naphtha in the dish then there are no floaters. Floaters float because there is liquid in the dish, if you remove the liquid completely how and where would they float?

Lol sorry, I maybe didn't explain properly. I understand that once the naphtha is siphoned, the liquid will be gone and the previous floaters are now at the bottom. I'm worried about them not sticking (so maybe they're more aptly called 'unstickables' than floaters at that pont), and once jar is turned over they will be lost.

I realize I'm being a bit anal, but hopefully that clarified things a bit...

 

[melotikaci]

Lol sorry, I maybe didn't explain properly. I understand that once the naphtha is siphoned, the liquid will be gone and the previous floaters are now at the bottom. I'm worried about them not sticking (so maybe they're more aptly called 'unstickables' than floaters at that pont), and once jar is turned over they will be lost.

I realize I'm being a bit anal, but hopefully that clarified things a bit...

Oh, I got it now
At that point crystals are wet and quite sticky so you shouldn't have a problem, but for precaution you can put a tin foil between the fridge surface and your dish and if any crystals don't stick and fall off you can recover them from the tin foil.
This is how I usually do it(not sure if elevation is necessary though):

 

[Portals2Eternity]

Lol sorry, I maybe didn't explain properly. I understand that once the naphtha is siphoned, the liquid will be gone and the previous floaters are now at the bottom. I'm worried about them not sticking (so maybe they're more aptly called 'unstickables' than floaters at that pont), and once jar is turned over they will be lost.

I realize I'm being a bit anal, but hopefully that clarified things a bit...

Oh, I got it now
At that point crystals are wet and quite sticky so you shouldn't have a problem, but for precaution you can put a tin foil between the fridge surface and your dish and if any crystals don't stick and fall off you can recover them from the tin foil.
This is how I usually do it(not sure if elevation is necessary though):

Ahh, I see. I'm so glad u took time to do this illustration! I was envisioning tipping at a MUCH greater angle, so now I see the crystals are much less likely to fall out, but the tin foil will take care of that if they happen to. Can't overstate how helpful youve been.

Just ONE last question, I promise! Shouldn't a lid still be placed on jar in freezer, and even outside freezer til container reaches room temp, to avoid h2O contaminating spice?If so, wouldn't this stop xtals from reaching tin foil?

Again, an infinite amount of thanks.
T - appx. 10days til Blast Off

 

[melotikaci]

Ahh, I see. I'm so glad u took time to do this illustration! I was envisioning tipping at a MUCH greater angle, so now I see the crystals are much less likely to fall out, but the tin foil will take care of that if they happen to. Can't overstate how helpful youve been.

Just ONE last question, I promise! Shouldn't a lid still be placed on jar in freezer, and even outside freezer til container reaches room temp, to avoid h2O contaminating spice?If so, wouldn't this stop xtals from reaching tin foil?

Again, an infinite amount of thanks.
T - appx. 10days til Blast Off

"h2O contaminating spice"? not sure how water will get to spice. if your fridge/freezer works fine that shouldn't be a problem.
I've never used lid after removing naphtha. :?
Anyway, good luck with your extraction :roll:

 

[Portals2Eternity]

Ahh, I see. I'm so glad u took time to do this illustration! I was envisioning tipping at a MUCH greater angle, so now I see the crystals are much less likely to fall out, but the tin foil will take care of that if they happen to. Can't overstate how helpful youve been.

Just ONE last question, I promise! Shouldn't a lid still be placed on jar in freezer, and even outside freezer til container reaches room temp, to avoid h2O contaminating spice?If so, wouldn't this stop xtals from reaching tin foil?

Again, an infinite amount of thanks.
T - appx. 10days til Blast Off

"h2O contaminating spice"? not sure how water will get to spice. if your fridge/freezer works fine that shouldn't be a problem.
I've never used lid after removing naphtha. :?
Anyway, good luck with your extraction :roll:

Does anyone else have a knowledge base re: close lid vs open, post-removing naptha, til container reaches room temp?

 

[downwardsfromzero]

Does anyone else have a knowledge base re: close lid vs open, post-removing naptha, til container reaches room temp?

Lid off allows water vapour to condense as ice in the container, but allows naphtha to start evaporating. Lid on brings risk of crystals redissolving in residual naphtha:

but if one were to use a container with screw-top lid it's possible, after draining off the bulk of the naphtha, to replace the lid and return the jar upside-down to the freezer and allow the remnants of naphtha to drain into the lid. The last drops of naphtha can be removed from the lid before allowing the closed jar to return to room temperature, then vent off the last naphtha vapours and collect the crystals. (Thanks to pitubo for this tip!)

 

[pitubo]

^^^ Ah, I see you beat me to it. :thumb_up:

A few more observations: while having water condense onto the naphtha-damp crystals doesn't do any harm per se, it does slow down the drying. Also, you will be amazed how much naphtha stayed put between the crystals when you see it accumulated on the lid of the upside down jar. Not having to evaporate it not only saves time, also all the impurities present in it will not contaminate the product.

In my experience, crystals that form through freeze precipitation are always stuck fast to the glass. They do not fall off, even when putting the jar upside down. If there are floaters in the ice cold naphtha, it is almost certainly ice snow and is a sign that the naphtha was wet or otherwise held tiny water droplets when placed in the freezer. If dmt crystals do come loose, you can reattach them by letting the jar warm up slightly (and as a result redissolve a small amount of dmt crystal in the warming naphtha) and replacing in the freezer. This will almost certainly glue the loose crystals to the rest of the crystal mass.

For the initial freeze precipitation, I always use a screw top jar, never a shallow dish. Scraping is not an issue, because I recrystallize anyway. After getting rid of the freeze precipped naphtha, the jar containing the crystals can be placed in a warm water bath and small bits of fresh naphtha are added until all of the crystals have redissolved. Any impurities that came over from the extraction, like bits of plant matter, base soup or lye will not dissolve, but stick to the jar. The solution can then be carefully decanted into a final crystallization container, which can be much smaller than the shallow dishes commonly displayed here. I just use another, smaller, screw-top jar.

If you are going to recrystallize the crystals anyway, you don't have evaporate the last bits of naphtha that remain after the upside down draining. It has no added value.

 

[Portals2Eternity]

Pitubo/downwards: ty! Exactly what I was looking for. Now, as I just became aware via acidic testing that my klean strip vm&p is no good, what is the best substitute? Im doing stb, nomans, and would like something, unless not wise, that would pull a full spectrum of alkaloids, rather tban simply n,n - as, to my understanding, heptane would...

 

[downwardsfromzero]

As a final straw, I'd make my own hexanes via the Kolbe electrolysis of rancid butter. Never had to resort to that yet, fortunately. For more sensible answers, you've probably seen my reply to your new thread (which ought to be merged back in here).

 

[Portals2Eternity]

As a final straw, I'd make my own hexanes via the Kolbe electrolysis of rancid butter. Never had to resort to that yet, fortunately. For more sensible answers, you've probably seen my reply to your new thread (which ought to be merged back in here).

Agreed.

And yes, ty for the many-a-response! Heptane it is. Any experience/knowledge you wanna share is of course welcomed.