How hot is your decarb step?
That’s super useful, thank you. In order to eliminate as much tubing as possible there are only two lines, one from the glass cow to the trap and one from the glass trap to the manifold. I’ll see about switching to a larger gauge of tubing.
The vacuum reads 160 or so without the cold trap attached, but that is at room temp, no process running.
The bar does appear to be moving, but there isn’t a terribly large amount of material in that 2l, about 300mg as a test. Is it possible that the area of empty glass is acting as too efficient a condenser, turning the whole shebang into a complicated reflux rig? I have a very large amount of flower, a very large amount of anhydrous ethanol, should I try with way more material or a way smaller flask (or both).
Decarb is 115c to stoppage of bubbling. Testing came with THCa below LOQ
You generally want your boiling flask half full, more if you’re doing second pass with the volatile removed. Insulate the the top half of your flask with fireplace rope. Wrap it around it like a coil. Make sure your stir bar isn’t to large for you flask it could be spinning but not at its target speed. Larger gauge of tubing will increase your pumps ability to pull a vacuum. But once again and I can’t stress this enough you need a better pump.
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300ml should still distill over. You should be running larger but in no case should you ever get your flask as hot as you are currently. If you don’t see anything by 200-210c just shut it off.
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I have a fiberglass tape with PID I use in other reactions that I could use as an insulator and perhaps even apply a gentle heat with that as well. Thanks I’ll try that.
With the pump issue, what about the better pumps remediates this situation? Other posts have seemed to suggest that 12.5 cfm is a bit overkill for 2l. Is this process simply not doable at 200-300 micron? Or is there another metric I’m not taking into account? This process working essentially lets me buy the more expensive stuff, so not having a great first or even second pass isn’t a deal breaker for me, I just need… well, any pass at all.
It looks to me like you’re dealing with two issues
First you’re under loading the system. Until you’re more experienced you should avoid under loading by too many % below 50%. Probably 25% full (1.25kg/5L flask) is the minimum I would do. This becomes more important with small systems.
Second when you are selecting a vacuum pump you need to look at both the CFM and the ultimate vac for the pump. You need the factory specs to be between 1 and 10 micron in my experience to have good success. Then select a CFM that will pull the system down fast enough. 3cfm pumps with a 1 micron ultimate vac will pull just as fast as 3cfm pumps with a 500micron ultimate vac. You might be able to get away with an Edwards8 on that little system.
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That makes a lot of sense. Do you suppose it makes more sense to extract 1l and put it into the 2l or get a say 500ml double neck and test say 250ml to give the pump less total volume to work with?
Which pump? if you get an edwards8 or edwards12 you’re in good shape I think.
Here’s the issue with under loading:
The environment around your system provides a certain amount of wind which cools the system. Cool distillation heads condense material in the head and drip it back down, preventing it from exiting the boiling flask. The glass sitting above the mantle starts cold so it has to be heated to allow material through. If there is no material in your flask there is no way for the glass to efficiently heat up and allow a fraction through.
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Got it. The heat that is very efficiently being transferred through the glass into the material is equally efficiently leaving the glass through the large empty volume. I didn’t realize the loss was so great but it makes sense explained like that. I’ll likely go with the E2M-12 you linked, I wasn’t aware the secondhand market was that much cheaper.
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Happy to help.
I’d also recommend looking around on eBay for a couple of days there are very good deals and sometimes they come with guarantees and with tested gear. This linked one looks only semi tested. You might want to look around more
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Sent you a PM
300 gram?
300mg is a big dab…if that’s all you loaded you aint getting anywhere.
(300ml. got it 
)
do you have a mantle that will fit such a flask. putting the wrong size flask in the mantle doesn’t do you any favors.
that pump you have will work with a smaller system, and I’ve heard tell of folks getting by above 500um
yeah, not enough in there…
you might also want to invest in a panda (cheaper than your pump). you’re leaving a lot behind with your current extraction.
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I would ditch the DOW vacuum grease and try some Apiezon grease instead.
It makes difference only on surfaces that get very hot such as the ground joint between the boiling flask and head and possibly the ground joint between the condenser and cow/swingarm (also if you have a ground joint on top of your head for the thermowell). Save your money do not use it anywhere else, you will not see much of a benefit if any.
(PTFE joint sleeves with a very thin layer of grease will save you a lot of headache and as long as you are gentle with them they will last for a very long time)
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Search on “devol” it’s not just about decarb.
“150C lake” might also yield valuable insights.
If you haven’t read I make terrible distillate....why? I suggest you start there.
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There is a decent SOP on extractorsolutions.com in the sop section.
might be helpful in your situation.
Success!
A few insights:
Underloading seems to have been the culprit here. I stuck with the current pump since the recommended pumps seemed to have similar flow and ultimate vacuum ratings. Came over at 240 microns, 170c at the head. Last and probably most importantly, we added a heat tape set gradually higher and higher, wrapped around the column of the SPD to help along the enthalpy of the system as much as possible.
I put it in a cart, color and clarity are wildly nicer than my expectations, as is the very neutral flavor. Sent out for potency testing just now.
I’m positive there’s gains to be made in vacuum apparatus efficiency. I’m going to try PTFE sleeves and nicer grease (thanks for the suggestions).
@cyclopath I’m reading up on devol thanks for the info. I’m also reading into best practices for setup of a panda, should have one by next week.
Again thank you everyone for your input, which has been incredibly valuable in this process.
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Great! Glad you were able to get some oil made.
Be ready for it to oxidize. It’s possible that you’ll be fine but in general oil made this way will quickly look like it’s bruising. It won’t harm the potency at all but the color is likely going to change. Maybe not though!
170C at the head is fine. What was the boiling flask temp?
Oh, good call. I have a big tank of food grade nitrogen I use to store volatile chemicals under inert atmosphere, I’ll get this in a more convient container and hit it with that.
Flask was at about 200.
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cheap upgrade: use oven rope wrapped around exposed flask instead of tinfoil. I think it insulates better.
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