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soxhlet exctracter

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you should be fine..

once you've basified the IPA, you've effectively made it more polar. if it's greyish, you've passed the titration midpoint (between pH 8 and 9) you're probably at a pH of 9 or 10, which is just fine. any higher, it will look black.
there should be two layers after adding heptane. keep both layers, but try to evap the heptane tomorrow (or crash it out in the freezer). you didn't ruin anything, the goodies are still there
 
I tend to go for straight to base rather than A/B.

Benzyme, Any idea why it stayed grey and at ph8-9 while there was still undissolved lye in it. Had it absorbed as much lye as it could? Anyway now I've added water with the rest of the lye its gone black. There are still 3 layers though - poss the middle one could be emulsion. I'lll drain them off later & that should give me a better idea.
 
Just an update, and a few questions. I did 3 pulls of 30ml Heptane, washing those with sodium carbonate then freeze preciping & 2 of 30ml Toluene. As far as yield goes I aven't weighed it out but after a freeze precip there isn't that much there visually. I'm going to lower the temp & see if more drops out but I think not al the goodies were pulled out by the soxhlet, probably it clogged. With the Toluene pulls very little came out at all, just a very slight waxyness & little sparkles, presumably DMT crystals, but it pretty much evaporated clean. Could this be due to the IPA not pulling out the jungle spice?

Is there any chance that I could have lost any spice doing the sodium carbonate wash, I don't think so but want to rule out all possibilities.

Also can someone confirm whether or not IPA pulls out all the jungle spice & other constituents of MHRB as well as DMT?

I've saved everything so I'm going to re-soxhlet the MHRB with some clean IPA once I get something to prevent the soxhlet clogging & discharging down the distilling arm which I believe is what likely happened. I'm thinking a hollow roll of fine metal mesh inside the soxhlet surrounded by MHRB, which someone suggested previously. I've got mesh handy so it shouldn't be too tricky. Also I intend to dilute the IPA with water before adding lye this time, any suggestions on volume of lye to use?
 
60g of bark was used, the most I could fit into the soxhlet. I added about 200ml additional water.

For the sake of completeness I should add that the coffee filter I used to drain the original sludgey IPA & heptane dried out and has absorbed a good quantity of spice judging by how sparkley it is. I'm going to chop it up and mix it in with the used bark when I re-soxhlet it.
 
69ron said:
...snip...

Another tip, if you powder your herb and mix it with a little diatomaceous earth (about 4:1 of herb to DE) for improved drainage, you can fit far more herb into the Soxhlet and extracting time is improved.

You’ll always need to put something to keep the glass connecting joints from sticking together. SWIM recommends using PTFE joint sleeves instead of joint grease (stopcock grease). PTFE joint sleeves are pricey but they last forever and aren’t messy. SWIM also uses PTFE tape sometimes (the kind used for plumbing). It’s cheap and not messy. Some people frown on that practice, but SWIM has used PTFE tape many times without any problems. He hates joint grease!

Yeah, I know, SWIM is a little opinionated sometimes. Sorry about that. SWIM is just not the "follow the crowd" kind of guy.
Click to expand...

Very good write-up 69-ron and great thread! :)

For mixing the herbs with clay, any specific type of clay, also more importantly this is by volume and not by weight correct?
 
4:1 is by volume.

The type of DE to use is the kind specifically used for filtering, the other kind makes things worse. The DE they sell for pool filters is perfect. It’s hard to find in “food grade” form though. Another option is cellulose at the same ratio. This can be more easily found in “food grade” form.

Another good tip is to wrap your herb in a handkerchief, as if making a burrito. Make the width just small enough to fit the Soxhlet will a little drainage space on the sides. This acts as a Soxhlet extraction thimble and works great if your material is not too finely powdered. Before loading the “burrito” of herbs, put something at the bottom of the Soxhlet like a glass ball or PTFE ball so that the “burrito” sits slightly above the bottom of the Soxhlet. This will help improve drainage.
 
Hi,

I just wanted to give you some feedback on my soxhlet issue and see if you can verify or shoot down a theory of mine based on observations of my 2 soxhlet extractions. The first one I've gone into earlier - it seems that the soxhlet had clogged. I improved drainage and re-ran the soxhlet with the same MHRB. All worked fine here - thanks for your advice - the soxhlet siphoned & plenty of alkaloids were pulled from the bark to the IPA. This was basified to a Ph of about 11 - where the IPA was black. I did pulls with Heptane (3), Toluene (1) and Xylene (2) with the latter 2 solvents still evaporating off and at present looking like they're heavily ladened with spice/jungle spice (apart from final Xylene pull which is pretty clear & is still in IPA).

Unlike the other solvents I did a Sodium Carbonate (anhydrous) pulls on the combined Heptane, as I'd done previously, on both occassions I noticed the following:
Once Sodium Carbonate wash was done subsequent washes with distilled water to remove any residual Sodium Carbonate were carried out. After agitation with the Heptane the water washes became cloudy, but in the sep funnel the cloudiness seperated out upwards. That is the cloudiness (presumably residual Sodium Carbonate) inside the waterlayer drifted upwards slowly forming a thicker whitish layer between the Heptane and the now clear water. Now apart from these 2 times using IPA as the initial extraction liquid I've never experienced an emulsion/whitish layer forming with Sodium Carbonate washes of Heptane. This leads me to speculate that it is occurring because of the fact that IPA was used initially - I can't think of any other explanation. I'm thinking that its possible something from the IPA was pulled by the Heptane in the soxhlet and is affecting the Sodium Carbonate wash. Does this sound plausible?

I don't know, as yet, if this is affecting yields from the Heptane but I have seperately collected the water used in SC/water washes and will evaporate this to see if any of it smells of DMT which would indicate I've lost some yield to the wash - presently it does have a solventy smell. I seperately collected the emulsion layer and heated it to try to get as much Heptane to seperate out as possible - this was pipetted out and added to the rest of the Heptane, the emulsion was returned to the IPA jar mixed with my final pull of Xylene - possibly I should have kept this seperate but I didn't see any benefit in evaping it off seperately as any DMT recovered could be ascribed to the heptane in the emulsion rather than to the cloudiness itself. I'm planning to evap off this Xylene and then seperate DMT/Jungle Spice from it later so I'm less concerned about the Sodium Carbonate (or whatever else the cloudy emulsion layer is) being in this than in my Heptane.
I put the recovered heptane in the freezer last night but nothing freeze precipitated out. I'm going to reduce the temperature as far as it goes but I would've expected at normal freezer temp to see something drop out. Its still yellowy though.

Has anyone (in particular Benzyme & 69Ron) experienced anything similar or able to shed any light on this?

One other, much more minor, issue I wanted to ask about is that after switching off the soxhlet the MHRB is still saturated with IPA, the same IPA which has been cycling through it collecting alkaloids. I'm thinking that a certain proportion of the alkaloids pulled out will be retained in the IPA saturating the MHRB. Can anyone speculate on the proportion lost here & whether there is any way to recover it - or even whether it would be worthwhile to try to do so. I'm speculatingthat doing a subsequent soxhlet on the same IPA saturated MHRB with water would be a possibility as this would wash out the IPA (and any residual alkaloids) leaving the MHRB saturated with non-alkaloid laden water instead but as IPA has a lower boiling point than water would this work? Is it even worth it?
 
The extent of the nerdiness that's going on in this thread here is delightful. I think I might have to get a soxhlet JFF. I might do some medicinal tinctures...
 
It seems that soxhletting with IPA pulls out more oils/fats than a normal mimosa hostilis basified water extraction. Just want to ask about the best method of cleaning this up & removing the oils. I expect that this is to do an A/B extraction on the soxhleted IPA but I've exclusively done straight to base previously. So I wanted to ask:
1) I understand the principle behind A/B but how is it possible to separate the acidic solution (and oils/fats) from the IPA with which it has been mixed?
2) Similarly what should be done between acidifying & basifying?
3) Is it better to dilute IPA before A/B, say with 50% water?
4) Are there any other soxhlet specific issues I should consider?

Sorry if these questions are a bit noobyish but I wanted to be extra sure this time.
 
1. you can't separate IPA from acidic aqueous solution because they're fully miscible. instead, use a nonpolar solvent like naptha to defat, before you basify.
2) same as 1.
3) doesn't really matter. the less water you use, the less volume you'll have to deal with
4)not that I can see, most of it has been covered. just a reminder, always make sure cold water is continuously running through the condenser.
 
Realy good information on this thread, made me buy a soxhlet.

Only thing I need to get is a hotplate... I narrowed it down to two choices and I would need your help to make a decision as I never used a hotplate before.
Ok, the first one: digital, porcelain top, max 325 C, 10x10 inch plate, stirrer
the second: analog, ceramic top, max 450 C, 8x8 inch plate, hotplate only
there's also another one which is stirrer/hotplate, aluminium with a temperature of 380 C.
What's the advantage of having the stir function?


Which one would you get:?
 
Get one with a stirring function, and one that's digital if you can afford it. You’ll regret it if you don’t get one with a siring function.

The best ones I've seen for the money are the Cimarec Digital Hot Plate Stirrers. They heat up to 540 C and are highly accurate. The 4 1/4 x 4 1/4 inch hotplate surface model is good enough for a 2000 ml flat bottom boiling flask.

When doing extractions, if you don't stir the contents continuously, it's more likely for the extractives to burn. Also, many solvents will bump violently if there is no stir bar present. Some people use boiling stones, but stir bars work better because they rotate all the liquid making the temperature more even throughout the solvent.
 
Thanks, 69ron!

I realised by now that the digital hotplate I mentioned is too large for my needs but I will definitely go for one with a stirrer.
Unfortunately Cimarec hotplates are very expensive and hard to find in the UK.
Do you think I could boil limonene with a hotplate that goes up to 380 C?
 
D-limonene boils at 176 C.

380 C is the surface temperature of the hotplate. Often that reading is just for a tiny point in the center of the hotplate. It doesn’t mean much. The contents in the flask will be below that temperature, and by how much is impossible to tell because it varies by the solvent quantity, flask type and size used on the hotplate.

If I recall correctly, with a 4 1/4 x 4 1/4 Cimarec Digital Hot Plate Stirrer that heats to 540 C, the 380 C setting is NOT hot enough to boil 500 ml of d-limonene in a 500 ml Erlenmeyer flask, but if using a small 50 ml beaker, about 220 C will boil the d-limonene.
 
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