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Distillation help

CrimsonRambeller820

CrimsonRambeller820

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Jul 12, 2020
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Maybe I'm in the wrong place for this, but there are 346 threads in the cannabis discussion forum at this time and the search tools do not point me in the direction where I'm trying to go. As my lab partner moves on to bigger and better things, I am having more control over the equipment. He insists about certain things however which I am trying to learn about as his way does not make sense to me. The top tempature gage he does not use because it beeps when it gets to 100c and he just turns it off at that point. The chiller always stays at 30c & in my opinion he starts collecting concentrate in the middle distillation flask way to early like out of the 3 flasks he rotates it to the main one we'll be collecting from after only a few drops into the first one. There is always dark distillate in the distillation flask when we're done and I'm not confident it won't be dark even after the 3rd pass. We've put a pause on this for like a week, but I want to know where I can find solid consensus on the questions I have about how the distillation apparatus is currently ran. The spin magnet is always being adjusted and he came up with the formula F(flow)=T(Tempature)+R(rotation/spin)+V(Vaccum)+C(cool)
Although usually I'm left feeling like I'm driving a car with the brake lines cut and the power steering out. We visually observe the 8-12 hour distillation process keeping the tempature on the mantle around 220-250c. I feel like there should be an exact tempature we need to be staying at, and I don't like ignoring the top tempature gauge because it beeps, in alot of ways I feel like thats the most important thermometer/tempature probe. I've been watching YouTube videos for hours and trying to see if I can find something anywhere that talks about the no-nonsense proper way to do it. If there's nothing wrong with what we're doing, why is the second cat so cloudy? Any tips or links to a thread where some of these questions have been answered already is appreciated.
 
Yes an internal thermometer will always beat external on the mantle. I don’t know the setup but surely it’s possible to get one that doesn’t beep? Other than that I don’t know shit on cannabinoid distillation but hopefully someone else does..

-GC
 
Is this for an oil extraction ...not quite following the procedure with 3 flasks...thanks
 
CrimsonRambeller820 said:
why is the second cat so cloudy?
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A visual indication is a poor man's way of testing for potency and often times inaccurate. Can you afford to send it into a lab for testing?

Most distilleries have a dedicated testing lab and use them multiple times for one batch of oil.
 
AussieJoe said:
Is this for an oil extraction ...not quite following the procedure with 3 flasks...thanks
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So, it consists of three single neck distillate flasks connected to the condenser where the idea is collect the crap in one, then adjust the base and rotate it to the next flask for the main collection, and then once it starts pulling over fats and lipids you want to adjust the base and rotate it once more to the final flask to collect that. The 1st and 3rd flasks won't be used. On this 3rd catalyst we're going to let the stuff collect in the first flask for alot longer than we have been before we move it to the second or middle. I believe rotating it too early is what's causing our distillate to look cloudy and polluted. Does that make sense?
 
w01fg4ng said:
A visual indication is a poor man's way of testing for potency and often times inaccurate. Can you afford to send it into a lab for testing?

Most distilleries have a dedicated testing lab and use them multiple times for one batch of oil.
Click to expand...
I'll have to ask, last I heard dude had a falling out with the guy who could provide the COA. If it's not 99% cannabinoids any percent seems to possibly indicate pesticides or something wrong with the starting material, although if the product is tested and comes out as 85% cannabinoids then it is also possible that the 15% that's not is some type of lipid or plant matter that distilled over.
 
G_Chem said:
Yes an internal thermometer will always beat external on the mantle. I don’t know the setup but surely it’s possible to get one that doesn’t beep? Other than that I don’t know shit on cannabinoid distillation but hopefully someone else does..

-GC
Click to expand...
The temp display on the mantle is from the internal probe in the boiling flask. The digital probe is at the top & is technically internal as it detects the physical tempature of the vapor right before it climbs into the condenser and precipitates down. That one is usually a lower temp than the mantle even tho heat rises. I'd like to get an idea on what temp is best for D9 to be at in order to distil, tho we end up using that digital probe as a plug because of the beeping when it gets past 100c. We should get a better digital thermometer that plugs into the top of the distilation head/condenser because I want one & it may be absolutely necessary like someone said visual observation is not really the way to go.
 
So if I were to take some crude that was made with ethanol and most of the ethanol rotovapped off & put it in the 2 Liter or the 5 Liter boiling flask, what tempature is best to set the mantle at? I'm thinking the temps may be different on the 2nd and 3rd catalyst. Whether that is or or not the case, I'm willing to do the distilation of 5 or two liters of crude anywhere between 200-275°c. Just asking again if anybody knows the prime temps for just the mantle, the mantle and the top of the distilation head, or one or the other, & if the amount of crude/distillate I'm working with changes what temps it should be at.
 
CrimsonRambeller820 said:
yes everything is under vacuum, what do you mean by the receiver?
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The glask/container that is going to be receiving/capturing your distillates. What vacumn source are you using if I may ask?

This is the last evaporator I used. I was recovering petroleum ether, methanol and ethanol in separate procedures. I had the option to use a powered vacumn pump but went with a tap adaptor b/c would cause far too many burps/bumps/boil ups. You have any activated charcoal or drying agents?

Tom
 
Thomas Davie said:
The glask/container that is going to be receiving/capturing your distillates. What vacumn source are you using if I may ask?

This is the last evaporator I used. I was recovering petroleum ether, methanol and ethanol in separate procedures. I had the option to use a powered vacumn pump but went with a tap adaptor b/c would cause far too many burps/bumps/boil ups. You have any activated charcoal or drying agents?

Tom
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Interesting. So no to answer your original question we do not use anhydrous sodium sulfate or calcium chloride. Also we are using a Dry Scroll vacuum pump. I have activated carbon and I'm pretty sure that's the same thing. When and why would I put anh sodium sulfate calcium chloride or activated charcoal/other drying agents in the collection flask, would that contaminate the thc distillate if I'm putting it in the receiver/collection flask? My buddy had used the activated carbon when I wasn't here but I believe he used it somewhere along the way during a butane hash oil extraction but that's completely different than distilation so I figure it's only worth mentioning briefly. Also Tom whatever you're doing sounds interesting and useful in the specific chemistry I am trying to do. Although I don't know what product you had to start with, having a Rotovap before I start any distilation not only to take some of the ethanol/ISO out of the wash/crude but to move into other chemical separations is good and makes me very happy. A final note I think the tap adapter would be good for a basic distilation set which I was going to start with but am very lucky to have access to very expensive equipment.
 
@CrimsonRambeller820 The. use of drying agents in the receiver is a) to help prevent an emulsion and to b) keep an anhydrous environment in the event of moisture sensitivity/stability.

Activated carbon is one and the same for my term.

I'm not doing anything. I took medical retirement. Working backwards I was a lab tech for a long time > graduate student in pharmacology/synthetic organic chemistry > degree in biochemistry/microbiology.

My education would have worked nicely for illicit purposes :cool:

Tom

As for contamination of the distillate, we would always just run further 'micro' distillations or use column chromatography or preparative HPLC or PrepSep cartridges for cleanup. The amount of mess I'd end up with would always depend on the number of synthetic steps or the difficulty of any given synthetic step.
 
Thomas Davie said:
run further 'micro' distillations or use column chromatography or preparative HPLC or PrepSep cartridges for cleanup. The amount of mess I'd end up with would always depend on the number of synthetic steps
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I understand what you mean. I will implement drying agents in my next run no problem, & trying to make good distillate by cat 3 should be easier even tho I'm not setting the mantle at a specific temp. I will do experiments coupled with estimation to see how much drying agents would be beneficial for a purer product. I'm doing more studying about this but my education is in no way formal. Therefore I'd like to ask do you think an exact temp is vital to distilation every time? I know how things have specific boiling points and melting points, so to distill a target ideally I am thinking someone would have to be above the boiling point but below the melting point. Anyway, thanks for your time and reply. If you click on my profile you can see from where I started in July 12 2020 with my first post and just on that you can see how much I've grown.
 
How 'exact' you hit the boiling point depends on the compound. For instance, a mixture of ethanol, methanol, petroleum ether and various unknown compounds from grain/feedstuff analysis would require fairly exact temperatures if you planned on recovering all
separate

40C petroleum ether (one variant)
64.7C Methanol
80C Ethanol

The length of the reflux condenser sometimes allow you to be more flexible, b/c a longer column will give a greater ease of separation. The best way I can put it is it sometimes allows you to stretch out or compress a distillation.

We had oen sauxhlet extractor that was four feet tall and always required 2 people to install it on a heating mantle.

Tom
 
Thomas Davie said:
How 'exact' you hit the boiling point depends on the compound. For instance, a mixture of ethanol, methanol, petroleum ether and various unknown compounds from grain/feedstuff analysis would require fairly exact temperatures if you planned on recovering all
separate

40C petroleum ether (one variant)
64.7C Methanol
80C Ethanol

The length of the reflux condenser sometimes allow you to be more flexible, b/c a longer column will give a greater ease of separation. The best way I can put it is it sometimes allows you to stretch out or compress a distillation.

We had oen sauxhlet extractor that was four feet tall and always required 2 people to install it on a heating mantle.

Tom
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Kool, great example. 🤔🤔 so different apparatuses for different jobs, and you'd definitely want to separate the components of a mixture if one was trying to get a pure isolated product. Me and my buddy talked about a Soxhlet but I don't remember how feasible it was in getting one, he mentioned needing five or something in order to separate all the ethanol out of the cannabis wash efficiently. I'll have to get back to you on that. So if I'm hearing you correctly, the yield between a short path distilation and the yield of the same distilation but with just a longer/more lengthy reflux condenser would be different?
 
The yield can be greater or lesser depending on the length of the distillation path, yes. For our solvent recovery apparatus in Animal Science, it was a fixed length c0ndenser. The variability would be in the temperature of the water bath, strength of suction and speed of rotation. Once or twice we had to use an oil bath for increased temperatures as we were trying to recover a high boiling point liquid.

Tom
 
Usually cloudiness is the result of either lipids or gums. Do you know if the crude was properly winterized?

If necessary you could dissolve 1 part crude to 9 parts etoh and drop temp to -30c at this temp all the fats and lipids can be filtered out, the etoh stripped and the winterized crude distilled.
 
Another possibility is that you have a vacuum leak and your mantle temp is set too hot for whatever is currently boiling. Instead of phase changing to a vapor your basically decomposing the product. This is called ghosting and you will see white smoke/vapor in the system.

Yeah if you're switching to the main collection flask to early Terps can also cause some cloudiness. This is where a vapor temp monitor is very useful, it can tell you pretty much without a doubt when your in the cannabinoid range which is usually around 185-195c depending on vacuum which is ideally under 100 microns. I never set the mantle above 220 personally.

You could also consider doing media washes with t-41, neutral alumina, activated carbon, or silica 60. these will really pull alot of pigments out but you also need to be aware of potential isomerization. I would avoid using them in the boiling flask or drying agents in the recieving flask.
 
Thomas Davie said:
The yield can be greater or lesser depending on the length of the distillation path, yes. For our solvent recovery apparatus in Animal Science, it was a fixed length c0ndenser. The variability would be in the temperature of the water bath, strength of suction and speed of rotation. Once or twice we had to use an oil bath for increased temperatures as we were trying to recover a high boiling point liquid.

Tom
Click to expand...
So in trying to recover a high boiling point material from a formula/mixture/product, is it as simple as looking up the boiling point of your target molecule; and then setting the mantle to that temp & letting it do its thing? If I'm correct in this part of it, what is the preferred device you would want to be sure reaches the boiling point of your target chemical- the mantle or the top of the distilation head/condenser?
 
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