Problem with my shatter, can anyone help me?

I'm pretty new to making shatter, so hopefully I'm just having some noob issues that someone can point out for me.
I do a QWISO which I then winterize for at least 48 hours.Then I put it in the vacuum chamber to purge. I've had success purging at a low temp (around 90 degrees F) as well as a bit higher (around 110 degrees F).
Lately though instead of shatter I'm getting this crumbly crap. It smokes ok I guess but it dries out and sticks to the silicone pad I purge on which takes away from yield, plus I hate the consistency of it.
I've taken notes on every batch I've made in order to establish a repeatable process that will yield predictable results, but it looks like I managed to fail at that since I keep doing it the same way but now I'm getting different and completely shitty results.
I did try a different solvent (99.8% anhydrous iso made for cleaning delicate electronics, seemed like it would be the cleanest solvent) so I'm going back to everclear and maybe 91% iso which have both worked for me in the past.
The solvent is the only change I've made to the process though. I'm wondering if I'm missing something and my successful batches were just luck and my process is flawed somehow. Is there anything aside from temperature that would give me that crumble instead of shatter? I'd really appreciate any advice.

Shatter is an oleoresin and crumble is a oil/wax hydrate. Look for sources of water and points of nucleation for hydrate crystals to form around in your process.

First question why are you winterizing a qwiso batch? Second question do you have a pic of end product? Im picturing the fully purged qwiso powder if thats case you should be able to warm it to liquid then let cool to shatter. Without a picture cant be sure if its nucleation or just qwiso

I see. The winterization process does bring condensation into play since the solvent goes pretty much directly from the freezer to the Pyrex pan to evaporate. That brings up 3 questions:

Would condensation be enough to cause a problem?

Since I'm using polar solvents which I believe are water soluble, would there be any visual indicators of trace amounts of water?

If this is my problem, what can I do to mitigate it?

Thanks for your quick reply btw!

If you're using less than 90% iso for that qwiso that's probably where the extra moisture is from. Or perhaps when frozen it's not sealed and the hygroscopic nature of the alcohol absorbing more water. Those are the two things standing out to me.

Sorry missed you did say you're using high %. I think you need to seal when frozen.

lio lacidem said:

First question why are you winterizing a qwiso batch? Second question do you have a pic of end product? Im picturing the fully purged qwiso powder if thats case you should be able to warm it to liquid then let cool to shatter. Without a picture cant be sure if its nucleation or just qwiso

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I'm not sure why I'm winterizing to be honest, I never get much of anything in the filters so maybe that's an unneccessary step. I don't have any pics but when it happens again I'll post some, that's a good idea.

gk skunky said:

If you're using less than 90% iso for that qwiso that's probably where the extra moisture is from. Or perhaps when frozen it's not sealed and the hygroscopic nature of the alcohol absorbing more water. Those are the two things standing out to me.

Sorry missed you did say you're using high %. I think you need to seal when frozen.

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I've used 91% ISO, everclear, 99% ISO, and everclear. I keep lids on the jars in the freezer for the most part, but sometimes not. Another great idea that hadn't occurred to me! It's sounding like winterizing could be the culprit here.

Yeah needs to be sealed in the freezer. Your just absorbing moisture the entire time. Sorry I rushed through that the first time and i guess responded before reading all of the first post. My apologies.

Id skip winterizing all together. Winterizing works very well with bho but is not necessary for qwiso or qwet

Yes I'll be cutting winerization out of the picture from now on. I do have a batch in the freezer now that I put in before starting this thread. Worse yet I left it in the freezer unsealed for a bit while filtering it after washing it. Sounds like I could be screwed in that batch but if it crumbles on me I'll at least take some pics and post them here.

I'll also post the results of my non winterized batch to follow. I'm curious now, is it necessary to put your solvent in the freezer before washing?

Thanks again for your help!

I alway froze my material and my solvent when I did qwiso runs

I freeze my material and solvent as well, use 99% ISO, or 95.5% EtOH.

No winterization, as polar solvents don't extract many non polar waxes. Iso more than Ethanol, because it is less polar.

I do seal winterization alcohol when I do BHO, though relative humidity in a freezer is ostensibly close to zero.

I evaporate most of the alcohol away using a rotovape, still, or heat mat, and then use use a vacuum oven at 120F and -29.5" Hg for final purge.

Ok, just wanted to make sure I had the part about freezing stuff for QWISO right haha. I'm feeling little silly for having to ask about this and especially for unnecessarily winterizing my QWISO like I was but thanks to you guys (or gals, hard to tell from screen names) I think I'm headed in the right direction. Very helpful!

Fadedawg, what temp do you use when evaporating your alcohol before purging?

I air evap with a fan 24-36 hours til it is a powder/crystally form then I scrape and put in chamber just warm enough to turn oil liquidy. Usually 100-120 depending on strain for a couple hours with qwiso runs

It only takes a couple of hours to purge? Theres another mistake I was making, I didn't let it get that dry before putting it in the chamber. I'd let the liquid evaporate but it was still kind of a paste or putty when I purged it, so it makes sense that any moisture I may have picked up along the way would still be hanging around to cause problems when I purged.

Fadedawg said:

I freeze my material and solvent as well, use 99% ISO, or 95.5% EtOH.

No winterization, as polar solvents don't extract many non polar waxes. Iso more than Ethanol, because it is less polar.

I do seal winterization alcohol when I do BHO, though relative humidity in a freezer is ostensibly close to zero.

I evaporate most of the alcohol away using a rotovape, still, or heat mat, and then use use a vacuum oven at 120F and -29.5" Hg for final purge.

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Correct though now I'm curious what the actual relative humidity levels are in a freezer. Think I'll check the standard -20, the frost free and then -80.

Like he said. Room temp. I always kept air circulating too, not sure if that's good or bad. Anyways so room temp for 24-48hr then would go onto just a run of the million heating pads for about an hour on the high setting to warm up the dish before vac'd.

Got it, thanks gk. I actually have air blowing on mine too when it dries. I used a 6" hole saw to cut a hole in each end of a 18 gallon or so tote. Then I ran the ducting from my fan/charcoal filter in my grow room into one hole and I got some duct coming out of the other one that carries all those alcohol vapors right out the window. It's pretty handy and I feel better with those fumes outside as opposed to floating around my house giving me a headache and possibly blowing me up. Plus its filtered air and I keep the tote clean so I don't have a bunch of dust or crap getting in my stuff which was a concern I had with simply evaporating outside.

Not sure if anyone gave a shit but measured the freezers for shits and giggles since I never have. As it would seem just by visual observation frost free is definitely lower, ~2%. Standard freezers were both close to 30% RH.

Well from someone who did refrigeration for years your freezer isnt running properly if its making ice on racks and walls like it looks in picture.