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
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.
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.
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
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.
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.
What do you guys think about using sand as a filtering agent?
I use alumina all the time as a winterizing agent @Stevesgoodsonline. 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.
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?
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 
.
Hey buddy so I have an in theory question on making an inline dewaxer with my CC
I’ve asked bvv they said yes should work
But I have a CC… Not cls … So if I get another open jacket column, stack under mine and put valve in middle and have guage on both columns, material top, inline dewaxer bottom…
Then since I have no nitrogen or closed loop, to move solvent from the top material column, to the bottom dewaxer column. But I’ll have gauges on each to see it move from one side to other…
And I can take my vacuum pump, pull vac through both, closing top column,then the bottom one, leaving me with negative pressure on each, and a valve in btw keeping them separate…
I’ll have to either get filter column or slide whatman slow filters in BTW viton gasket filter on each side…I know this alot info bare with me… So the negative vac will allow me to fill top and soak, then move to bottom with negative pressure left on bottom column, open valves watch it move on gauges, and if not moving good since I’m backyard, maybe take empty cans and use the gas left to move it on to the bottom if any Is left… Then I can cryo soak and evacuate.
Would this basically be a inline dewax column then? Do you think the negative pressure will move the solvent ( along with jacket column temps being colder?)
The guys at bvv told me I might be on to something… Does the idea sound feasible, does anyone know anyone that tried this
Good input. Seems like something that I am going to have to play around with and see what happens 
gotta love fresh ideas and having no clue if they will work or fail hahaha
I like your idea and I think I’m following what your idea is and why you want to run it.
By pulling a vac in both chambers when introducing the solvent the vac will assist pulling solvent into the system. Similarly when you open the ball valve to dump your solvent from material column into dewaxing column the negative pressure will assist the movement. However people who use this same method in their cls sometimes have issues clearing all of the solvent from the material column to dewaxing column and this is called vapour lock. I am not exactly sure what causes it. I have seen people say that they can even start pulling vac on their recovery chamber with all valves to column open so they would stop and assume that they have recovered everything, but when they open up the system to the atmosphere they find a noticeable amount of solvent that has been trapped in their material column. This only seems to happen when running columns at cryo temps. This is why people often use nitrogen assist because it is the only reliable way as far as I’m aware to clear your loaded solvent out of your material column. In theory any gas should work to force the solvent through but use a gas WITHOUT any oxygen! Gots to keep the conditions inside the columns safe so no chances of explosions
So your theory should work but I would be looking into a cheap nitrogen cylinder and regulator kit to help you out. Also because when you are filtering your solution leaving your dewaxing column you will need positive pressure to assist the movement of the solution through the filter which nitrogen is perfect for. As said elsewhere if you try and pull the solution through the filter as opposed to pushing it , you will cold boil off your solvent and damage your vac pump. Although I seem to remember you saying you used water aspiration to pull vac so I guess that isn’t really an issue for you.
Hey buddy thank you so much for actually reading that! Yeah so that’s me only issue was wondering if it would have pressure to go on through the filter, it goes through it when there isn’t another columm in the middle but yeah…ok so the gas in the can contains oxygen…hmm ok that means using it dangerous huh…
Ok how much nitrogen does it take, will a quick, pop of the valve be enough? Yeah if there is another big hidden cost I’m going back wards…
I’ll finally be able to get my solvent colder -40f , this may help about grabbing plant matter, seems like if I soak it any it starts grabbing plant matter… Looks like I gotta get the cryo column back out too… Just so next easier to set it in dry ice with it piled around it… Thanks so much again…
Also I have water asiparted vacuum for my buchner funnel, I really wasn’t planning on pulling on it but before I loaded it with Tane
So i guess you will have to give it a go and see if it works without adding positive pressure. You can add the pressure by adding warm solvent vapours to the top of the system but then you are using more solvent and not sure if the warm gas would counteract the cold winterising proccess.
I just bought 10lb of brown alumnium oxide for use in winterization of ethanol thc extract, before evaping then into my distillation rig.
Albeit only 20.00 or so for 10lbs.
I hope I have the correct product. The celite 454 I didn’t hear about until today.
I have gone through pounds and pounds of alumina. I found 220-240 grit to be about right. I have used finer grit but much finer that 400 grit and it makes more of a mud and is hella slow to vacuum through. I used to be able to get white alumina but can’t find it in abrasives anymore. No difference but the color looked cool in a column.
Alumina as a filtration agent is very hard to beat. Essentially it is very old tech and is simply a sand filter which are highly efficient irregardless of application. The alumina is often used in chromatography so there is a great body of knowledge to tap on the sites that deal with chromatography. There are TONS of peer reviewed articles and posts dealing with its use in chromatography. As you pointed out too it is dirt cheap lolz plus it is inert and can be cooked way hotter than is possible without a kiln before heat impacts it at all. You can cook it very hot. It fact one lab I did was to cover the extract in a layer of alumina in my sublimator. Then I tried to see if I could cook the gas up out of the alumina.
It was a very early stab at research and the alumina just popped dust all over inside as the extract bubbled but the point is that it is a very versatile compound.
I’m a smaller scale patient, trying to make very small batches of RSO with the equipment that I have available at home (equipment: MB2E, heated magnetic stirrer, sink aspirator, Buchner filter and a counter-top domestic still). My goal is to improve the final medicine by removing the lipids, waxes and chlorophyll; but, I’m unsure about a few steps, as my starting point will be an ethanol extraction from the machine (aka nasty dark tincture). If anyone can review this and give me some feedback, that would be greatly appreciated!
UPDATE: Thank you to everyone who has responded. If you also have a MB2E, do yourself a favor and read the threads on here. The cold ethanol extraction tek is a much more streamlined process that results in a far superior end product. No comparison…
Dry Ice Assisted Cold Ethanol Extraction for RSO
Ditch the butter machine and use cold solvent so as not to pick up any of that stuff. See Bucket Tek (Cold Ethanol Extraction on a Budget)
You can make 70% THC with essentially the tools you have, even with only a -20 Freezer. Effective meds. Dabbable or edible