BKM for Evap and Scraping Post Freeze Precip

[Triptic]

BKM - Best Known Methods

So after the latest freeze precip I have come to the conclusion that I suck at post freeze precip procedures. Figured this needs to be worked on, and who best to ask for advice than the experienced?

To start, upon pulling out the latest freeze precip there was fair share of nice white xtals. Quickly poored out the excess solvent, and set up to evap with a cool fan to blow on it. Two things quickly happened, condensation appeared appeared all over the Pyrex dish obviously due to the change of atmosphere from the freezer to the countertop. Second, the xtals all went kinda transparent like, I am assuming turning to a goo. Could still see little bumps where the nice white xtals were, they just weren't pretty white anymore.

Poored some hot solvent back into the Pyrex dish in hopes to re-x them, but a thin film that had developed with the evap seemed to not want to disolve back into the solvent.... Scraped some of the film up in the solvent with a blade which pooled up some yellow blobs in the solvent. Curious to how long contents should take to disolve back into the solvent, is that thin film something to worry about, would the dmt have disolved back into the solvent while ignoring the film? Currently have it back in the freezer for another 18 hrs to see what happens.

So finally the scraping. Currently I use two blades, a razor blade and a small blade similar to an exacto knife. Goo I am at a complete loss on how to scrape and get into a holding vessel. Sticks to the blade, but how to get it off the blade and into a collection container has me perplexed. Xtals, though, seem to break up and leave trails of powered xtals across the surface of the Pyrex dish. Eventually getting what I can scraped up of the xtals, powdered and hole, get some nice lovely white spice stuck to the blade... Which tends to have a little freely fall off into the collection vessel, the rest remains stuck to the blade which I then use the other blade to scrape those xtals off the original blade. Basically going back and forth from blade to blade while trying to get the xtals to lose their hold and falls into the dish.

In conclusion I figured I would make a thread to see how fellow travelers conquer these tasks. Compile a list of best known methods that I can hopefully apply to my experiences to better perfect my technique and solve some issues I have had in the post freeze precip activities.

Thank you much, and look forward to reading your woes, successes, and honed techniques.

 

[alert]

I looked at some of your previous posts and it seem like you are doing an ACRB extraction.

Sadly, I don't think anyone has found a way to get crystals via freeze precipitation. You will get crystals at first, but as they come to room temperature they will inevitably turn into a goo.

The only way I have seen people getting crystals from ACRB is letting their solvent get super saturated and letting it sit at room temperature after decanting. Many people are able to get crystals to precipitate out of the solvent at room temperature and they don't melt back into a goo for whatever reason. These crystals tend to be waxier, but at least they are in a solid form making them easier to work with.

So finally the scraping. Currently I use two blades, a razor blade and a small blade similar to an exacto knife. Goo I am at a complete loss on how to scrape and get into a holding vessel.

You can either rub the goo directly onto some plant material to make enhanced leaf, or you can dissolve your goo in a minimal amount of IPA or acetone, transfer the liquid to your holding vessel, and let the solvent evaporate.

I have read of one person who said their goo crystallized somewhat after being dissolved in IPA letting the IPA evaporate off but I'm not quite sure why that would work.

There is some good discussion in this thread about how to obtain crystals from ACRB

The other thing you may try to do is dissolve all your goo in a minimal amount of hot naphtha so the solution is super saturated and see if you can get crystals to crash out at room temperature. If you are lucky you may get some and they won't melt.

 

[Triptic]

My first extraction, though a fraction of what the possible yiels can be, came with 200mg or so of nice white xtals. This was after several freeze precips of excess solvent as I did not evap enough prior to the freeze precip. Got them in a small jar in the fridge for safe keeping. I am wondering if my latest go around was more a result of condensation absorbing into the xtals changing them to goo more so than a lingering bit of solvent in the spice.

You are correct in that I am using ACRB, 50g a test run. Going to try throwing the dish in the fridge post freeze precip before bringing to room temp to try and slow down the climate change and hopefully reduce the condensation.

 

[3rdI]

Hello triptic,

I have never used ACRB but my post FP method with MBRB Is as follows.....

1, Remove pyrex tray from the freezer and pour off the solvent through a filter to catch any floating goodies.
2, Trap a filter between the tray and the lid and put it back in the freezer upside down and on an angle for 30-60 mins to allow the remaining solvent to run off into the filter.
3, remove tray and place vertically against a wall and blast with a fan for 30ish mins
4, once completely dry scrape up the goodies
5, :shock: :surprised :d

 

[The Day Tripper]

Heptane?

Is it selective enough to get xtyal's from acrb?

IF so, i'd recommend a hot water bath, to get a small glass shot glass of heptane boiling, and dissolve what you can of your freebase in that.

Get an airtight seal on it with 2 rubber bands, and some tin foil. One around the rim of the shot glass, then put the foil cap on, then another rubber band.

Put it in the freezer, and when its all crashed out, pull it out, and use a pipette to transfer the heptane into another shot glass.

Then put your shot glass with the crystals in it, in a mason jar with some anhydrous epsom salts, google as far as making anhydrous epsom salts. Let it get to room temp in the sealed jar, so no condensation occurs, then open it up to evap the residual heptane present.

Scrape with a razor blade, small metal rod/paper clip/whatever.

Works great for me, but thats my tek for re-x'ing what i get from mhrb. Don't know how it would work for acrb, but its the bees knees for mhrb freebase.

Then you just evap your heptane until its milky. and repeat, until theres no heptane left.

It will give dirtier crystals each time you evap off some heptane, and freeze it again, but its the best method i've tried.

 

[Triptic]

3rdI - Good idea on the flipping tray upside down after decanting excess solvent post FP. Will give that a shot. Never have issues with condensation when returning to room temp and evap, or does having tray upside down with fan blowing on it help with that?

The Day Trippet - Only have naphtha at the moment. Does the salt absorb moisture, thus preventing condensation issues?

Thanks for the wondetful info. Keep it comin peeps!

 

[The Day Tripper]

3rdI - Good idea on the flipping tray upside down after decanting excess solvent post FP. Will give that a shot. Never have issues with condensation when returning to room temp and evap, or does having tray upside down with fan blowing on it help with that?

The Day Trippet - Only have naphtha at the moment. Does the salt absorb moisture, thus preventing condensation issues?

Thanks for the wondetful info. Keep it comin peeps!

Yep, the epsom salts in the mason jar act as a dessicant/drying chamber.

Give it a try with naptha, it might work! :thumb_up:

The shot glass method, using super saturated naptha/heptane is a very good way to freeze-x imho. Its just a little tricky working with near boiling hot heptane/naptha. Make sure you have good ventilation, and are using an electric hotplate/water bath.

You could also put dried epsom salts in a ziplock bag, and put a flat dish with your crystals in that after you drain it, after pulling it out of the freezer. Just be careful not to get any epsom salts inside the pyrex dish. Should prevent any condensation as the glass warms up.

 

[hobobrown]

Kind of what Alert said about getting the pulls super saturated and let the crystals fall out at room temp.

Or super saturate by combining pulls then reduce by evap before freeze precip.

Doing this option, I determined, that if you have decent ACRB ratio among the alks, that the dmt is so abundant as to engulf the goo and hold into at least a paste form which eventually dries out. Then you'll have a nice dry mixture that is yummy. Although, goo isn't bad either if you can find a good way to store it.

Have a pic below of combined pulls that were saturated, evapped, and freeze precip.

Notice goo in the middle? It was dried out by the morning.

 

[alert]

Doing this option, I determined, that if you have decent ACRB ratio among the alks, that the dmt is so abundant as to engulf the goo and hold into at least a paste form which eventually dries out. Then you'll have a nice dry mixture that is yummy. Although, goo isn't bad either if you can find a good way to store it.

My theory concerning the issue of some people getting a goo that refuses to crystallize and some getting crystals and/or a goo that will crystallize has to due with the ratio of NMT : DMT and whatever other alkaloids (b-carbolines?) may be in the original source material. Some people have pulled beautiful shards out of room temp naphtha that weren't active at all so I think confusa definitely has a alkaloid profile we don't completely understand yet. I've read the ratios change depending on the time of season the material is harvested as well. I know some people have used trunk bark/stem bark likely has it's own slightly different alkaloid composition.

As far as the goo, like you said as long as you can find some place to store it, it is fine. Quite potent as well.

 

[3rdI]

3rdI - Never have issues with condensation when returning to room temp and evap, or does having tray upside down with fan blowing on it help with that?

I have never had any problems with condensation, it happens but it just runs down the tray and pools at the bottom.

 

[Triptic]

Upside down evap seems to be the way to go for me. Leaving to conrinue the evap til morning after work to scrape. Propped, upside down, fan blowing, and towel covering. Think I will give a 100 g extract a shot next. Lookinin good at the moment, an even mix of xtals and goo. :thumb_up:

 

[Entheogenerator]

Sadly, I don't think anyone has found a way to get crystals via freeze precipitation. You will get crystals at first, but as they come to room temperature they will inevitably turn into a goo.

I almost always freeze-precipitate using NAPHTHA and ACRB and haven't had any problems getting crystals. I don't think the precipitation method is what determines the consistency (crystals vs. goo).