Winterization


#82

Isomerization is normally caused in an acidic environment. Magnesium Silicate is slightly alkaline.


#83

When you say crystalline silica are you referring to crystobalite and quartz? I was researching celite 545 distributors and after reading the MSDS’s it appears that many of them contain between 30 and 50% crystalline silica in the form of crystolaite and quartz such as the millipore celite 545.

The best I could find was from Honeywell which claims less than 1%.

Just trying to get more details because silicosis sounds like no joke.


#84

if you freeze over -40 c how many hours do tou have to keep it at that temp to filter everything in one filter


#85

so it doesn’t if it isnt food grade . i was going to buy in pool supplies way cheaper didnt because it was’t


#86

So food grade DE is safer to use for medicine but there are just so many types and grades that it can be difficult to decide what to use. Main problem with regular food grade DE is the particle size is usually too small and does not help filtration much. The problem with pool grade filtration DE is that it may contaminate your medicine with heavy metals such as arsenic or iron. Arsenic is a poison and iron will promote oxidation of your distillate. Also, watch out for PH as dE can be acid, neutral or basic. You may not realize but isomerization may come from your acid activated DE. Who knew!


#87

The simple answer regarding health is to read, understand, and follow the MSDS. DE is used by some to eat just like carbon powder is. If you read an MSDS for the particular product you are holding and it warns of say arsenic or warns not to ingest then don’t. The MSDS for clean sand warns against exposure and avoid ingesting for example but understanding the rest of the MSDS gives you generally enough info to otherwise decide for yourself how to use it safely.

The key concept here is very simple - if you are not certain it is safe and know precisely why or why not it is safe then avoid it until you are certain. Removing stuff from the compound never creates a toxic situation in and of itself. The same cannot be said for adding into the compound so should be approached from that viewpoint.

“Safety First” was what the man taught me in the Marine Corps on the grenade range… of course he was referring to removing it before tossing the grenade but it is about the same thing, right? :flushed:


#88

What would happen if I took my fully saturated mix the moment it come out of the column and ran it through a buchner funnel slow paper. I’m already dewaxing in the column… But I’m still picking up some plant material when I soak to get everything, could I not immediately it run it through the Buckner since it’s cold and since this supersaturated and not evaporated any then I wouldn’t filter out any of the thca ,is that not correct, using a water aspirated vacuum… I don’t want the thca to be filtered out and I know if I put the cryo Timbs with any evaporated out it would crash out then be filtered out and I would rather not do that that’s why I said I fully saturated mix but nothing has been evaporated out of yet


#89

Vacuum won’t work for this type of filtration. The Vacuum will instantly boil your butane. You need pressure to push it though rather than trying to draw it through a filter. https://www.opensourcesteel.com/products/os-buchner-vessel
You need something like this, it goes in between your column and your collection pot.


#90

Why does adding 2 whatman slow paper before and after the metal filter not help any? Like directly inside the column

And thank you I didn’t think about it boiling the butane, say even if everything at cryo temps the water will heat it right?

Could an extra column be added with filters to get it off the material, I just don’t won’t the THCa to be filtered out either


#91

It is because of blow by, remember when you had a hard time seating your filter paper? It’s like that, only inside a column. Yeah a filtration column would work.


#92

Ok with filtration column, can I simply just add another to the bottom mine, with some sort separation valve, then move it into the next by opening valve, or would it need special pump or something to aid into moving from one column to next… Guess what I’m saying is can I out fit my closed columm to do this for the mean time…

Without special pumps

And it blows by even if they clamped in, that sucks, guess I gotta figure out this second column…I don’t wanna use any other solvent


#93

You can add it below your column inline with a ball valve. Drive it just like a passive system. You can use nitrogen as well to push everything through.


#94

Back in the good old days I used to use a vac assist to filter my single solvent (butane) winterization (not ethanol) through a fritted Buchner funnel with a coffee filter inside to prevent clogging of frits.

It’s pretty much a frustrating process and I don’t recommend it at all but if youre determined to do it, it’s possible.


Only The Strong sauce tek
#95

Would pulling vac on both sides,top through the bottom, close the top, continuing pulling on bottom, then shut bottom, then both top and bottom would be under vac, only fill the top, then close top, would the negative vac on bottom be enough to pull it to the next side? If so would this work, I’m not CLS just closed column


#96

How were you able to draw it through the filter without boiling it? I can almost boil the solvents I filter and they are much longer chain hydrocarbons.


#97

Alright guys nobody try this at home. These were open blast days…

Pre chill Mason jars w solution in a cooler lined with dry ice blocks. Place a dry towel on top of block creating a barrier between jars. Ideal chill temp to prevent thc crash. You will know you crashed your thc if you see a dark oil patty on the bottom. The crap should look like green brownish sand.

Also pre chill your glass Buchner, receiving flask and a 2 liter measuring cup ( my favorite lab glass lol)

After about 90 min ( don’t quote me on that) you can begin filtration.

Pull a vac on a vessel such as a stainless steel "honey pot"or vac chamber. I recommend having cold traps in between the pump and vessel. If you don’t have a cold trap make sure you’re in a safe ventilated area.

After the vessel is at full vac, close the valve to pump and connect your vessel to your buchner using barbed connections. This can be done before hand if you have more than one vac port on your vessel. But we want that glassware to be cold up until the last second.

Pour your solution into the measuring cup. Leave measuring cup on dry ice for 2 min to allow crap to sink. You should have a crystal clear solution with crap on bottom. (I wonder how it would go if you poured while still cloudy.)

Fractionate your solution into your buchner by pouring slowly leaving solids behind. Open the valve on your vessel very slowly experimenting with flow rates. I find just barely cracked open is the way to go.

Bam!

I found that the fractionating technique from my measuring cup saved me a lot of headaches and I eventually just poured solutions into clean jars leaving behind fats (and thc oops) and leaving behind my buchner.

Some things to watch out for would be not only having clean glassware, but also completely dry. If you flush with isopropyl followed by water, Make sure to get that water out. The butane will hit the water and instantly ice up creating a blockage.


very clear bho shatter (Definitely scammed) !!Warning to all hash lovers and makers!!
#98

What do you guys think about using sand as a filtering agent?


#99

I use alumina all the time as a winterizing agent @The_Goods. 220-240 grit seems to work just fine. Alumina is the “sand” on most sandpaper and a layer at least on top of a glass frit will keep the frit from clogging.

Alumina is highly effective at filtering out “wax” and can also be used to catch chlorophyl if you swell that stuff up first by boiling in rubbing alcohol as 70/30 iso to water. It works better than anything I have tried and I have tried them all. I have come to believe that sand from our apartment volleyball court would likely work just as well really. I use that sand for chromatography lolz and no worries but that is used in tiny layers to protect silica gel.

The problem with my example of volleyball court sand, or fish tank sand and so forth is not so much what it is made of but really that I have no source of such uniform size grain sand. The volleyball court sand is strained by me to get the big chunks out but otherwise the grain size is all over the place. More to the point the grain size is typically pretty big compared to the say 240 grit alumina I get. So while alumina is not sand per se it is a great idea in my opinion to switch to using a filter like that because I do it every single batch. In fact I have learned that prewetting the alumina with tap water can further enhance the seperation of waxes in a big way. If I had access to 220 grit sand from the beach all nice and clean and screened for uniform size then I would certainly try it.

If you prewett just about any flter media, even you paper watcom filter, you will enhance the seperation capability of waxes. My bet is that if I did take the time to screen the sand for uniformity and get it clean and prewet it with water then the seperation power to stop waxes would be likely about the same as alumina sand. Clean up is also a breeze and in fact that is how I stumbled upon this great technique. I was tired of scrubbing my glass frit after dewaxing. So I thought why not just put a layer of sand on it so the mess will build on that and then I can just scoop it out? So I had some alumina grit because it is sold as abrasive and I kept some around. I put a layer on and tried it and was astonished when I saw how much more effectively the waxes were halted at the top of the layer. It did indeed end my days of scrubbing glass frits too!

Good idea.

Alumina is found in the abrasives section of Amazon. It comes as brown or white and either type works identically. At times you can find activated alumina which is fine too. “Activated” means simply that the stuff has been cooked in a very hot oven and similar treatment in order to increase its absorption power like in a chromatography setting. This would not be relevent to winterization at all because it is gonna be deactivated lols the moment you prewet it which is frankly the entire point! Activated alumina is precisely what you need if for chromatography because it needs then to be VERY dry or it throws off the mobile phase.


#100

So much useful info as always @Beaker! But with more knowledge comes more questions…

You say that alumina should be prewetted before use as a filter. If using to filter fats from a cryogenic butane solution then would the moisture in the alumina freeze and essentially block the filter? Could it be prewetted with something other than water to prevent this from happening?


#101

I have zero ideas about how this would work with a cryogenic mobile phase. Water would seem completely incompatible at first glance as you are pointing out.

This is probably a case where you just have to do it to find out what problems are gonna present themselves. I have been a part of multiple engineering projects from concept to customer delivery of some very sophisticated robotic motion control stuff for factories and mills and such. I learned with certainty that on a new project there is simply no way to anticipate the problems you are going to need to solve. In that case you just make your best guess and go for it lolz.

At times things go boom, or bridges collapse, or the Space Shuttle does blow up, but generally that is the way engineering is done. You make your best calculations, best judgements, and best effort then hope the boss is not present when the purple smoke starts coming out of a six figure machine slated for delivery in one week and already six weeks late…

My delayed thinking suggests that if you pursue this as you reminded me water may well be a huge factor for you. Therefor my input into the project would be only use activated alumina which is what I destroy by adding the water. I forget how hot they have to cook alumina to get it REALLY dry but my oven my home goes to 550F and as I recall the figure was above that at least a hundred degrees or so. Kiln temps.

I have found that even the slightest traces of an unwanted solvent say in chromatography can throw everything off to the point it is a fail. Tenths of parts of one percent by volume imo will change the way it plays out. If that notion carries over to your project then tiny traces of water in unactivated alumina would also impact it. Just a hunch here but that is why they go to the trouble of baking it lolz although I have only ever heard of activated alumina being a necessity in liquid chromatography as I might use it. I suppose you are building an LC project but one at radically different conditions than ambient so … liquid is liquid no matter the atoms but that suggests that any other liquid you use needs also to be only liquid at those conditions. The trick then would be to find solvents with a wide polarity difference but that both dissolve the THC and do so one better than the other.

Then you would have a mobile phase you can tune in like manner to DCVC. I better vape one more bag though before I edit more… my head hurts :flushed:.