Extraction Apparatus w/ Laboratory Glassware

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deep buddy

deep buddy

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Need a run down of your extraction process to best answer this question.

For me I'd simply distill the stuff over under vacuum. You may lose some terpenes/flavor doing this without a vacuum--and you may lose some anyway with one if you are not careful and do not know the identities of the terpenes in your strain, some will be more volatile than others.

Anyone doing ISO extractions industrially would benefit greatly from a rotovap imo--there just isn't a better machine for the job. Also because you're going to be using the reclaimed iso for further extractions purity should not be a huge concern. Any impurities you'll have will all be weed related. Now if you want pristine iso back, it complicates things a lot but if you're just trying to save on your solvent bill--I'd go distillation.
im doing a quick wash iso extract using cold iso. really basic just iso over material filter then evap w/ or w/out heat.

i would assume that if i used a lil heat and vacuum cold trap i could get most of it. the solvent stays very clean thru this process.

hehehe roto-vap hell yeah i wish i had one of those but... i am building a chest freezer unit that will automate a majority of the process
 
squiggly

squiggly

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Yup just get yourself a nice big boiling flask, a sparkless hot plate (with stirrer is a nice addition for many odd jobs you'd probably never think of using it for I'd be glad to point out), a distilling column, and something to catch the crap. Put the receiving flask into an ice bath.

The hot plate is really where the splurge is here--a sparkless one (which you absolutely need) can be pretty expensive. A nice one is definitely expensive. Mostly universities and research labs buy these so of course they are appropriately priced (1000% mark up).

You can probably get all of the glass for 2-300 bucks maybe even cheaper.

If you wanna go vacuum you need to get heavy-walled boiling flask, and make sure everything else is rated for a vacuum--most of it is tbh. It will be more expensive.

You could presumably build a "cold finger" system except instead of an open area below the finger you'd have a place to collect solvent. This might take some engineering ingenuity--not my strong point, see Graywolf :)
 
Graywolf

Graywolf

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hey squigs and Gwolf . im really interested in solvent recovery systems. i have a good enough extraction process that im really happy with i just want to recycle my iso. what do you guys think would be the easiest method?

thanks in advance Deep

Hi DB! Sorry to just find this, but the forum has been spotty during upgrades!

For recovery of the alcohol, I don't think you can beat the cheap simplicity of a pot still.

Regardless of whether you use a pot still or a more elaborate and spendy Rotovap, you won't be able to finish off in either, because you can't see what you are doing with a pot still and you can't get the finished oil out of a Rotovap flask without using a solvent.

The solution with both, is to reduce most of the alcohol in the still or flask, and then transfer it to another device that you can see what you are doing and easily remove it after reduction.

Here is my own cheap solution, using locally available parts:
http://skunkpharmresearch.com/alcohol-reclaim-still/

For alchemy, you can't beat glassware, and most of ours was donated to us by supporters, but the rest we have gotten on line, from American Scientific, or have had custom made at a local scientific glass shop way cheaper than list.

Though way cheaper than list, minimum orders are required, so we've placed orders with them, when we had enough stuff to meet minimums.

A boiling flask, an Alhin condenser, and a separatory funnel are the three key pieces I would recommend building from. An elbow and a Graham condenser would be a good addition for distilling

As SQ notes, a stirring hotplate is a keen addition, albeit spendy, and I further recommend getting one with an integral stand if you can.

I would check out E-Bay and Craig's list first for scores, before pundling up any cash for new stuff.

Skunk Pharm Research doesn't sell glass ware, but when we place orders, some of the local pharmers tag orders onto our order.

One who does that and retails them to patients cheap locally, is [email protected]. If you are down to buying new, you might check with her before paying retail. Depending on timing, and shipping costs to your location, she might be able to save you money
 
Graywolf

Graywolf

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You could presumably build a "cold finger" system except instead of an open area below the finger you'd have a place to collect solvent. This might take some engineering ingenuity--not my strong point, see Graywolf :)

Still working on our solvent recovery under vacuum. Thus far, it is less than with a simple pot still, because we need more condensing area than I got running an ice water cooled Alhin and a Graham in series, with two ice water cold traps.

Sorry the new forum platform isn't letting me post pictures, but I will when that is sorted out.
 
squiggly

squiggly

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Still working on our solvent recovery under vacuum. Thus far, it is less than with a simple pot still, because we need more condensing area than I got running an ice water cooled Alhin and a Graham in series, with two ice water cold traps.

Sorry the new forum platform isn't letting me post pictures, but I will when that is sorted out.

Have you tried different solutions for ice baths?

I would first try using a salted ice bath to get around -10 C. However there are other options available, carbon tetrachloride and dry ice will give a nice cold ice bath--in fact just google dry ice bath and you'll find a page ( a wiki i believe) which will outline a number of different solvents for dry ice bath at various desired stable temps.
 
squiggly

squiggly

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I think if you're doin enough bulk losing a bit off the sides won't matter as it'll be continuously recycled into the next batch. Should be able to get most of it out with heating. Either way, even if flipping to a vac chamber there's no simpler way to reclaim solvent.
 
squiggly

squiggly

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Except for the part about getting it out of the flask afterwards. Maybe start with a rotovape and finish in a vacuum chamber.
Also worth noting that glass isn't the only rbf material used. There are PTFE rbfs out there and perhaps even some substrate affixed polar surfaced flasks. PTFE would be a close place to start.
 
Aerojoe

Aerojoe

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I have included some crude pictures of the apparatus, please forgive my artistry (or lack thereof).

einl8i.jpg


zmiae1.jpg
I'm not sure how these invalid links work? but they never work for me. do they work for others? links say invalid and that I got wrong page some how, but it's always this way 4 me w/ these links. any help is appreciated.
 
squiggly

squiggly

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These images were posted before the THCFarmer revamp--I'm assuming they were lost in the process.

I'll be presenting my current research this week and next so it's a busy time for me--finals soon to follow after that, have a couple weddings to attend--you get the idea. I'll come back to this thread some time in May and get an updated diagram posted--sorry for the inconvenience.

Any questions, get at me.
 
squiggly

squiggly

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Except for the part about getting it out of the flask afterwards. Maybe start with a rotovape and finish in a vacuum chamber.


I realized while working in the lab today that my professor has already solved this problem--it should've hit me sooner.

Peep it:


Normal 20120413 00042
Normal 20120413 00044




He has essentially reduced the 20/40 connector down to a cap (with proper seals) with a hole drilled through the top to allow the vacuum to be pulled. As you reduce your sample down you can add more until you've reached the desired weight--you'll want to keep the sample container less than half full to avoid bumping.

If you haven't invested in a rotovap yet graywolf--may I offer a suggestion that you are missing the hell out. These bad boys are useful for just about everything. Even just to heat a sample up without the vacuum--it's a huge time saver in many ways.

And no that is not BHO in the rotovap. You would not want to smoke this stuff :)
 
squiggly

squiggly

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I was thinking of this being a solution to package it in vials. I see many folks with this stuff in similar vials anyway. I.e, take it out with a dabber :) These vials are cheap and represent a good packaging method imo.
 
Graywolf

Graywolf

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How much can you get in a vial by this method and still have it act as a thin film evaporator?
 
El Cerebro

El Cerebro

1,197
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rotovap are kinda $$, no? Seems like maybe could be a motorized diy for the part that rotates then connect to standard vacuum pump? What sort of fitting do they use for the moving part?
 
squiggly

squiggly

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I'd say somewhere near half-to-three-quarters full if you play with the angle on the motor arm. This stuff is viscous--but if you're applying enough heat to loosen it up a bit, it will leave a "trail" of a thin film to be evaporated as it spins. You don't necessarily need to keep the sample size small enough such that it's only enough to coat the sides with thin film, so long as you can take advantage of viscosity in leaving a trail.

Yeah rotovaps are expensive--but can be had used for not the most extreme amounts. I am positive that graywolf could engineer one around the requisite glass pieces that'd work perfectly well.

Really, though, for someone like you gray I see this as an easy way to speed up your vac purge.

Slap on a 20,000mL flask, rotovap the thing, apply heat while you're spinning (at an exact temp through water temp control, another benefit of this setup) to cut the viscosity. Dump out as much as you can (should be a lot if you're doing high volume), then add alcohol dropwise to strip the rest--vac purge that fraction using your normal method.

Any time something needs heated in the lab (which isn't going to produce a mild or violent reaction), I'll throw it in the rotovap at normal pressure. It really is a great way to heat something to an exact temp.

I use it when working up reactions, and for doing dishes (rather than sit and swirl sulfuric acid in a flask for 5 minutes--i toss it in the rotovap to spin it for 2 with heating).
 
Graywolf

Graywolf

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I've certainly looked hard at the Rotovape and it would be easy to engineer one, using a simple rotary union, but most of our oil goes into sublingual medication, so we just cook off the solvent and decarboxylate in the same step, making vacuum un-necessary.

Our simple vacuum chamber does an stellar job in the small quantities of carboxylic acid cannabis products that we produce by thin film vacuum purging and it is easy to remove afterwards.

A Rotovape is on the wish list, but the used Perkins Elmer Gas Chromatograph that we just picked up was way higher on that list, because we are tired of shooting blind and relying on only anecdotal information. I under stand how a GC works, but there is zero chance that I could ever engineer one myself.

Next highest on our wish list, is the rest of the equipment that our biochemistry student requires for his tissue culture, synthetic seeds, DNA sequencing experiments, and fraction distillation separating the stream constitutes by refractive index.

I would grab a Rotovape at a price I couldn't refuse, but in retirement am on a fixed income and have to pick and choose toys. We hope that eventually Skunk Pharm Research lease program income will pick up that slack and start to support more and better toys, so I can start to spend my own monthly mad money allowance on other thangs.

Maybe take my tolerant and supportive wife mate on a wild weekend wearing golf balls as big as diamonds for instance.
 
Graywolf

Graywolf

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263
this thread went over my head pretty fast.

Things in the mirror may be closer than they appear brother SP! Google Rotovape and ye shall be enlightened.

It is just a device that spins a boiling flask of solution on its side in a hot medium, and the thin film that adheres to the inside flask wall as it rotates up and over the top, is purged in a thin film by the vacuum that the system operates under.

It does the same thing a thin film in a Petri dish does, just way faster.
 

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