Freeze Precipitate Crystals Not Sticking

[Neo-Shaman]

I recently did a MHRB extract using Cyb's TEK. However, for some reason, the crystals, which I can very clearly see in my jar after over 48 hours in the freezer, are not sticking to the jar itself. They simply float around in the solvent like a bunch of little beads. There is a lot to! probably about 1g worth of product. But, I've never had this happen. should I try to filter the crystals? One time I tried to filter using a coffee filter and that didn't work at all. If someone knows of another filter or perhaps why this is even happening let me know. Below are some pictures taken after a Re-X and then a heat bath to rid of excess solvent. The picture before it was placed in the freezer, as you can see, is extremely cloudy and saturated once it had cooled.

 

[BongWizard]

I don't do a lot of freeze precips personally (partially for this reason). You can try evaping your solvent a bit more (even evap it while freezing) or your other option is filtration. You can use a coffee filter, but the xtals will stick to the paper and you'll need to recover them with acetone.

Here's another idea that just came to me; drop a small piece of broken glass into your solvent and allow it to freeze overnight. With any luck, your xtals should grow on the sharp edges (just had the thought that maybe there's no room for nucleation in your jar).

 

[NotTwo]

To be honest it looks a bit mucky and difficult to work out what are crystals and what's impurity. I'd let the solvent evaporate off completely then go for getting fluffy white(ish) crystals as follows:

1. have your product in a wide flat bottomed glass container
2. place in preheated hot water bath (no flames or heat needed at this stage)
3. add minimum solvent and stir until all soluble part dissolves
4. let it cool slowly checking on it every 20 mins or so
5. at some point you'll find little puddles of yellow oil forming on the bottom. the solution may also start to go just slightly cloudy - don't let it cool any more than this before going on to 6
6. pour off the solution to another wide flat bottomed glass container. all the puddles of oil and other solid matter will stay on the bottom of the first container
7. watch pretty little crystals start to form for 4 or 5 hours
8. put into freezer to make sure every last bit of spice crystalizes out
9. pour off solvent and leave to dry
10. use a thin piece of card to scrape off the crystals on to blotter. using a metal blade means you scrape up a thin fatty layer that usually settles on the bottom.

 

[Neo-Shaman]

To be honest it looks a bit mucky and difficult to work out what are crystals and what's impurity. I'd let the solvent evaporate off completely then go for getting fluffy white(ish) crystals as follows:

1. have your product in a wide flat bottomed glass container
2. place in preheated hot water bath (no flames or heat needed at this stage)
3. add minimum solvent and stir until all soluble part dissolves
4. let it cool slowly checking on it every 20 mins or so
5. at some point you'll find little puddles of yellow oil forming on the bottom. the solution may also start to go just slightly cloudy - don't let it cool any more than this before going on to 6
6. pour off the solution to another wide flat bottomed glass container. all the puddles of oil and other solid matter will stay on the bottom of the first container
7. watch pretty little crystals start to form for 4 or 5 hours
8. put into freezer to make sure every last bit of spice crystalizes out
9. pour off solvent and leave to dry
10. use a thin piece of card to scrape off the crystals on to blotter. using a metal blade means you scrape up a thin fatty layer that usually settles on the bottom.

Oddly I was attempting this as you posted it! I Re-X and the solvent is considerably clearer. I was being lazy and only did one Re-X before. I was going to let almost all the solvent evap in the heat bath before removing it to cool and evap at room temp. Will update soon!

 

[Neo-Shaman]

I don't do a lot of freeze precips personally (partially for this reason). You can try evaping your solvent a bit more (even evap it while freezing) or your other option is filtration. You can use a coffee filter, but the xtals will stick to the paper and you'll need to recover them with acetone.

Here's another idea that just came to me; drop a small piece of broken glass into your solvent and allow it to freeze overnight. With any luck, your xtals should grow on the sharp edges (just had the thought that maybe there's no room for nucleation in your jar).

Thanks for the quick reply! I'll have to try this seeding with a glass shard. I believe it to be plausible since the jar is very well rounded.

 

[cyb]

Some questions...

1. What is your solvent?
2. How cold is your freezer?
3. Are you Positive it's MHRB?

They're an odd colour.

 

[BongWizard]

Some questions...

1. What is your solvent?
2. How cold is your freezer?
3. Are you Positive it's MHRB?

They're an odd colour.

Don't tell me you've never smoalkd a bit of ooey gooey Cyb

You've got a point though, does look a bit fatty (yellow) for a typical MHRB extract. Excess fat could be the (un)sticking point.

 

[Jaffster]

Are you using Naptha?

Because it should be clearer than that, if so I guess you might have pulled the emulsion along with/instead of the Naptha.

 

[Neo-Shaman]

Some questions...

1. What is your solvent?
2. How cold is your freezer?
3. Are you Positive it's MHRB?

They're an odd colour.

1. NM&P Naptha
2. Food storage freezer on the coldest setting. Other extractions have freeze precipitated quite nicely. (But I have had problems with freeze precipitation in the past, in general.)
3. Pretty sure, I've used the same bark with phenomenal results before.

 

[Neo-Shaman]

Update:

So I Re-X'd one more time and placed the jar in a cool dry area to let cool and evap at room temp instead of freeze precipitating this time. I believe my problem to have been water/condensation inside the jar from opening the lid frequently to check on crystal growth. As well as my use of finely powdered bark this time. My bark is shredded in larger chunks. On my last extracts, I simply cut it into smaller pieces to fit inside the jar. This time I used a coffee grinder to finely grind the bark to a powder. This resulted in many more tiny contaminates in my solvent during pulls than the comparable clear solvent I pulled off bark extracts in which I did not finely grind up my bark. Which in turn caused me to do more Re-X'ing. However, Having to go back has made me realize something. I've decided I will always do a room temp evap first in the future. The extra time it takes is definitely worth the rather beautiful crystals that form. I took pictures of the saturated solvent as it evaporated and posted them below! In the last one you can see these beautiful crystals with a layer of yellow gooey solvent on top. I wrapped the jar tightly in a clear food wrap with a rubber band and placed it in the freezer to freeze precip' any remaining spice in the Naphtha. Will post some pics of the finished product! :want:

P.S. there are about 5-6 black dots in the last picture before I placed the jar in the freezer. These are from the rubber stopper on my syringe I used to pull solvent. I'm a bit of a perfectionist so I'll be getting those out soon.

 

[BongWizard]

P.S. there are about 5-6 black dots in the last picture before I placed the jar in the freezer. These are from the rubber stopper on my syringe I used to pull solvent. I'm a bit of a perfectionist so I'll be getting those out soon.

These bits of rubber contamination are caused by excessive wear on your syringes due to degradation from your nps (don't worry, I use plastic syringes for top pulling, too). To avoid this in future, before using the syringe, coat the inside with a silicon based lubricant (I use silicon grease for glass to glass unions and silicon lube [READ: anal lube] for any joint involving polymers).

As for the xtals, you've definitely got plenty of spice there, but it's loaded with what appears to be fat (even with reX). You should try fractionating your crystals. What I mean is, place your DMT laden solvent into the freezer and allow to cool for 3-4 hours (you should see the fat congealing at the bottom of the jar) then, pour the cooled solvent into another jar (preferably one that been precooled) and continue to freeze to precipitation.

Alternatively, you could do a mini A/B to remove the fats and a simple evap should yield snowy xtals.

 

[cyb]

but it's loaded with what appears to be fat (even with reX).

MHRB has little to no fat onboard (that's why I was suspicious). It's not like ACRB at all.

Also the 'jelly' looking substance is odd...only time I've heard of that appearing was when someone heated the base mixture excessively and it migrated to the solvent.
45-55C is all that's needed.

Yes...mini A/B will sort it all out.

 

[DansMaTete]

Yep, it definitly looks like exces heat. I had the same problem with my first extraction. A mini A/B is more efficient than a re-X to get a better result.