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soxhlet size

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GnicGnoc

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Hey, trying to decide on what a good size soxhlet extractor would be. I've never seen one in person so I'm having a hard time visualize the capacity of the extractor body. If I'm going to be working with around 100g to 300g of material would something with an upper joint of 70/51 or 60/45 "1000ml soxhlet" be good. I don't want it to big or to small, but just right:wink:
 
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neat, you have inspired me to make cocoa my next project. If you have any more info that would be nice. Would the alcohol pull the cocoa butter as well? If you have any suggested reading material I would also appreciate that.

Edit*
I was doing some reading and it seems most cocoa powder has been pressed and butter removed? So I guess I wouldn't have to worry about butter being pulled?
 
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Standard Hershey's cocoa, and pretty much all brands of cocoa powder, would indeed be defatted; I suspect the full-fat stuff is generally referred to as cacao.

Benzyme said:
theobromine precipitated at room temp, as an opaque, waxy, white mass
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Interesting. This sounds a lot easier than the messing around I've been through when extracting caffeine from tea leaves.
 
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benzyme said:
yea. the solids are likely a theobromine/cocoa butter mixture.

nothing to it, really. just cycle 190 proof alcohol for 6 hours.
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Hehe I did that once. I was extracting blackberries with azeotropic ethanal for a moonshine. simple setup: 500ml fbf on a hotplate. I had some imcredible bumping that caused my 300mm alihn condemser to hop around before cementing a 3' wide bright blue/purple stain on the cieling.

Good times.. (The stain is still there)

I also did some using raspberries/gourmet white chocolate. After the alcohol cooled to room temp I set it in the freezer overnight. I had large offwhite waxy precipitate.
 
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Once I finish my kratom I'm gonna move on to cocoa/cacao and play with both. Honestly I'm just looking for an excuse to use a new piece of equipment.

Have any of you guys ever used spirytus rektyfikowany (rectified spirit). I had a small bottle of it a few years ago and it worked nicely for a mushroom tincture, seems very clean.
 
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GnicGnoc said:
I remember when I was a kid, parents always told us not to feed chocolate to dogs. I guess maybe the theobromine is the reason why?
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You guess right.

Thanks for the safety reminder, ND!

Now, speaking of safety, I'm just contemplating how that's a pretty big soxhlet set up to be playing with. Larger amounts of hot flammable solvent are relatively more dangerous than smaller ones. Maybe you should consider going for a smaller soxhlet as well, GG. For one thing, when conducting a smaller extraction you'll want a smaller boiling flask and you don't want to risk it boiling dry.
 
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It is quite massive, the upper joint on the body is around 100mm and I can fit my hand all the way to the bottom. I understand the concern for safety but I do take precautions. My work area is well ventilated and fire extinguisher on deck. Still I would like to get a second smaller soxhlet for experimental runs.
 
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I have my 500 ml soxhlet & all the support gear. I want to make MHRB tea with it, but after a couple hours of searching it's not clear if I should use vinegar with the distilled water as my solvent. When I would brew in a pot I used vinegar but the soxhlet can run for so much longer, perhaps I don't need it? I'm thinking of letting it run for 48 hours. I've read many soxhlet teks and they all use 99% IPA, methanol, or 190 proof ethenol (Everclear) with the goal of making smoke-able crystals. I want fair tasting tea, that's all. Can you advise me on vinegar or no vinegar and soxhlet run time, please?
 
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markbraniumx said:
I have my 500 ml soxhlet & all the support gear. I want to make MHRB tea with it, but after a couple hours of searching it's not clear if I should use vinegar with the distilled water as my solvent. When I would brew in a pot I used vinegar but the soxhlet can run for so much longer, perhaps I don't need it? I'm thinking of letting it run for 48 hours. I've read many soxhlet teks and they all use 99% IPA, methanol, or 190 proof ethenol (Everclear) with the goal of making smoke-able crystals. I want fair tasting tea, that's all. Can you advise me on vinegar or no vinegar and soxhlet run time, please?
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IMO you can pre-soak MHRB in hot acidic water, then put it all in Soxhlet along with some fresh water. This is called Randall-Soxhlet extraction.

Vinegar will work fine as some acetic acid will make it through the Soxhlet I guess, even though it won't be needed due to presoaking.

Also IMO you don't need Soxhlet for water extraction as I found just three to four 30 min cookings are enough to get most of MHRB in the water. I found filtering using cheesecloth followed by loose cotton & vacuum sufficient and easy enough.

I haven't had much success with ethanol extraction of MHRB in Soxhlet (low yield for some reason), but since you have 500 ml Soxhlet, alcoholic extraction may be worth a try.

Here is a soxhlet tek from Trickster:

So, after many trials and errors here is my best Soxhlet or CSLE tek.

1. Soxhlet alcohol extraction (methanol and ethanol seem to be better than IPA).
2. Distilling and drying the alcohol as much as possible.
3. Dissolution of the extract in diluted phosphoric acid (pH ~4.5).
4. Settling/decanting/filtering the acidic solution.
5. Basifying to pH ~11.5 by adding diluted NaOH drop-wise and checking pH regularly.
6. 6-7 small Heptane/Hexane pulls. Prior to pouring the mixture into a sep funnel I stir it for 10-15 min with a mag stirrer/hotplate on "low" and temp set on 50 C. I prefer Hexane because of its lower b.p.
7. Reduction of NPS until it becomes cloudy. Usually to 1/3rd - 1/5th of the original volume.
8. Slow cooling of hermetically sealed freeze-precipitation beaker. 2 hrs at room temp + 4 hrs in a fridge + 8 hrs in a freezer.

The procedure has been tested several times and it consistently produces ~1% yield. The product looks white and crystalline. No MP test yet, but bioassay results are very positive. 3 different persons were launched into hyperspace using 30 mg each.

Advantages:
- efficiency (most of alcohol and NPS could be recovered),
- consistency,
- high yield,
- eco-friendly,
- good quality product (no need to re-x).

Disadvantages:
- requires some special lab equipment,
- requires certain minimal skills.
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I also found IPA (IPrOH) to be inferior compared to ethanol and methanol. 190 proof works as well as 200 proof, methanol is probably superior but quite toxic (not if the product is dried properly, rather higher risk of interchangeability with EtOH).
 
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