You see this guy’s sublimation rig @BreakingDabs
Other methods for removing water is the use of heptane or Alkane in general. As far as testing, I assume this is a preprocessing method, I was wondering if the products had been ran in a wfe and spd side by side to see if there’s any isomer changes based on the procedure. The water on alumi concept is genius
@BreakingDabs They (Whatman, et al) make even simple gravity filter papers that are hydrophylic and hydrophobic, based on whatever filtering you need to do. It is a brilliant idea, honestly, but you can easily make your own, even by accident, using other media, too… if you pour water over a cotton ball in your funnel, then pour the entire volume of a water w/ supernatant non-polar partition over it, all the water and stuff it’s carrying will flow through the cotton ball and the non-polar (such as hexane, toluene, and all its stuff) will stop right on top of the cotton ball as if it were a solid plug! @Beaker I love the fact that you are using grit as your alumina source! Check out sandblasting materials at Harbor Freight for bulk. But if you want pure laboratory grade white alumina, you might want to try Jaxon’s stuff: http://www.jaxonfiltration.com/Activated-Alumina.html
Using Cotton balls to help with filtration
@Future I recommend you leave the link to that split topic up in this thread, permanently if you can. I know sometimes there are settings for them to disappear after a certain time has elapsed, but it makes sense for it to be here.
I take my crude BHO and dissolve in 3:1 Methanol (highly polar) to Oleoresin. Run it through a Buchner at room temp through 220 grit Aluminum Oxide. I then add 4:1 heptane (non-polar) to oleoresin to the methanol oleoresin solution and blend well. I prepare my brine wash 4.0 ph in the correct quantity for the amount of oleoresin and pour the methanol-hexane-oleoresin into the brine wash. The methanol and all water solubles completely crashes into the brine water and leaves only the oleoresin heptane solution. Mix for 10 minutes and onto next step… The water comes out dark pink. I use methanol because it is inexpensive and the SOP for safe handling is the same as for ethanol. This saves a lot of time. Alternatively, if you are extracting with ethanol, the same results seem to occur with extracting with methanol and then going directly to mixing with Hexane and crashing in brine. Methanol is inexpensive and easy on the pocket book to throw out with the water.
As @beaker has pointed out methanol doesnt form an azeotrope with water or ethanol making it extra handy.
Yes. Methanol and Ethanol are very close in boiling point etc. Denatured alcohol also works well. 801% methanol and 20% ethanol. No excise tax! Amazing to see how the methanol oleoresin crashes out of the heptane and carries all the water solubles with it. Yes, if you use methanol for extraction you get more chlorophyl but they all crash out with the methanol in brine wash.
Have u tried the degumming process after extraction? the heat and carbonic acid formation can cause the lipids to break down in a similar manner to the citric acid degumming. maybe doing a post extraction degumming will remove that gunk
That may be okay for small quantities, but methanol is rather toxic and cumulatively dangerous, so wear an organic vapor mask and hope it works for methanol fumes.
Respectfully, I have a different perspective of the safety of methanol. I believe it is one of the safest solvents in use and I have seen hundreds of gallons used. Lots of people use it as fuel.
Methanol as a racing fuel is used pure on the sprint cars I used to pit for. The stuff is splashed all over the place in that chaos. It is also used extensively by RC model folks. I have used it from Torco as RC racing fuel for a long time. It gets handled by amateurs this way for fuel and solvent to clean parts and such all the time. (I am not suggesting for one minute that a sprint car pit area is a safe place but it was the best example I had )
A rag wetted with methanol cleans a lot of things pretty well. I have not noticed undue safety hazards of the fume. It will burn your nostrils if you take a whiff down close to the boiling vessel but you won’t be able to inhale it at exposure levels that cause harm because the body will gag if you try. Yuck. Methanol burning engines are notorious for the fume they produce and that fume is like tear gas lolz but if it is not being burned in a fuel rich combustion chamber then methanol won’t do that. The burning fume from a methanol burning race car will sting the eyes of the crowd badly if the wind carries it over them and it will bring tears to the eyes of the crowd hehe.
I appreciate the safety aspects of solvent but I believe methanol to be at least as safe as the other solvents used. No sparks around it although it’s fume is not particularly volatile compared to acetone (nail polish remover) or hexane (which smells like gasoline). Keep good room ventilation for all solvents and you will be fine. I keep a 6” carbon filter unit meant for grow tents running in my lab area at all times as well and when evaporating into open air the room is open to fresh air.
Methonal is about as dangerous as acetone. They both break down in the liver into nastier components. Ventalation is very important in a lab, it keeps you safe. PPE like gloves, safety glasses prevent exposure. Does your filter vent outside?
AEGL-1 for methanol on the air is 670 ppm for 10 minutes, 270ppm for 8 hours…
As little as 10ml ingested is toxic. Chronic skin contact is toxic.
Effects include permanent blindness, neural damage, and death.
I am still dialing in but have run it from 1400-3500 with varying results the temp is at 115 . Have a hard time running it any cooler than that . Interesting I’ve heard good things about aluminum oxide . What pore size do you find has the best flow rate ? I’ve read different things on carbon but one of them is pulling heavy metals through and compromising your oil .
“hard time running it colder” literally or like hard to justify? cause co2 below 1500 psi doesnt benefit from higher temps do to co2’s weird quadrupolar solvent properties. and at or above ~2800psi co2 is polar enough to pick up chlorophyll. i use a sintered stainless steel disk that doesnt really come with a equivalent This is what ive read in multiple scientific papers and it matches well to my experience with co2.
I dont really worry about the particle size or flow rate to much i just extract as normal. its at high enough pressure that only well compacted sub 2 micron particles will really hold that pressure back. you can take pressure readings from before and after and as long as the pressure delta between them isnt to large then your good.
ADS-3 Influence of Adsorbent Size.pdf (858.1 KB)
i use Super-Small-Particle-Filtering Stainless Steel Porous Discs
"Also known as sintered filters and frits, these discs have tiny holes that trap super-small particles. Discs are often used in laboratories and gas-bubbling applications (sparging). They’re Type 316L stainless steel for excellent corrosion and abrasion resistance. Select discs based on the size of the particles you wish to remove. For example, talcum powder is 10 microns in size. "
“Available For Particle Sizes- microns 2, 5, 10, 20, 40”
Literally the systems capabilities lean towards running it hot . The lowest temp I’ve been able to run the extractor is right around 102F . What kind of parameters do you find most successful(extractors/seperators)? I’ve also played around with the separators a bit but don’t want to adjust too many variables at a time . I am new to co2 extractions and have a system that’s not fully dialed yet . I am trying to get away from a co-solvent with co2 as it seems to be far to aggressive in the extraction stripping the material of just about everything . The idea now is to go from a co2 extraction to a QWET to get the remainder of the cannabinoids. Very interested in implementing these disks in the process how do you have them fitted to the vessels ?
the first one i used had a custom bracket that was screwed into a blind hole but ive also done it with just standard washers
Im going to opposite direction and increasing the cosolvent percentage while extracting below zero f
I do love sintered stainless! It clogs easily with low pressure or vacuum applications, but it is made for high pressure.
yes but isnt “gets clogged easily” just another way of saying filters really well ? lol