Sohxlet Extraction

[Windswept]

So, sort of a still, and will be used in parallel with my still! I got a soxhlet extractor for christmas this year, and I'm really looking forward to trying it out! Does anyone on here use one to make flavouring agents for their shine? I'm thinking my first run will be with coffee, then who knows what! I still have a bunch of chicory I picked this fall that I'd really like to try.

[Single Malt Yinzer]

That's GINORMOUS. Most Sohxlets are tiny. I want to get one for extractions but I haven't yet. Have fun with that and post up what you do with it. I'm interested.

[Windswept]

So I ran it with some fresh ground coffee and about 500mL of feints (around 60% ABV) for 24hrs as a test/cleaning run. I had some issues with using a crock pot water-bath as a heat source, so I'm rejigging things to use a hot plate and sand bath.

End product, about 400mL of jet-black coffee/alcohol mixture which has really strong coffee/burnt molasses/heads smell and about 5mL of coffee oil which smells a lot like soya sauce!

I've ordered a vacuum still and I'll try and pump up some vodka as high as it will go for the next run and see what happens. I can also use it to separate the solvent from the product!

Anyways, pictures!

[OtisT]

Subbed.

What is the target temp or range of temps needed for the bath? Just wondering if a sous vide cooker would work for that. I’ve been cooking with one since Christmas and damn, does it work well.

Otis

[Windswept]

Subbed.

What is the target temp or range of temps needed for the bath? Just wondering if a sous vide cooker would work for that. I’ve been cooking with one since Christmas and damn, does it work well.

Otis

I ran it on high, which worked out to 95-97C, quite a bit of a range. It worked ok, but the crockpot had an auto-off feature so it shuts down after 9hrs.

It just needs to get above the boiling point of your solvent (ethanol in this case).

I thought about a sous-vide or instantpot, but I’d still have an issue with evaporation if my water bath. I think with the flask buried in a pot of sand with a hot plate, hooked up to a temperature controller I’m ticking all the boxes.

Welcome to suggestions though.

[OtisT]

Thanks. I may try something like that with my sous vid unit then, so save some up front costs of embarking on a new hobby. I know it will run up to 204 F. I can always make pure ethanol so I only need ~172 F. I’ll have to check out my units max run time.

My 13 year old boy is interested in extraction of oils and I thought this would be a cool way to introduce him to the hobby of distilling without the idea that he is making alcohol to drink. My dad taught me distilling at about the same age, but for me the connection came because I was excited that I could burn the resulting product. It’s a different world these days.

I’m just damn excited that my son and I could actually have one similar interest to share, especially now that he’s a teen.

Otis

[Windswept]

Here's the new setup, I've included a temperature controller since this picture so I don't have to fiddle with the controls as much. I used peppermint for this run from leftover tea bags.

[richard1]

That's a great sohxlet and RC. Where did you get them from for the lab still. Have seen a lot of smaller ones but not this size.

[Windswept]

That's a great sohxlet and RC. Where did you get them from for the lab still. Have seen a lot of smaller ones but not this size.

My brother got it for me, but based on the shipping time, it's probably from China. I've had to buy a couple of bits for it, and had really good success with Deschem on ebay.

A lot of the other stuff is from the dollar store, cotton pads, glass beads, etc.

[Windswept]

And gleaning back the alcohol, I didn't get it all yet, but it was fascinating to watch the glass reflux work and how clean the alcohol comes back out. Just a hint of chlorophyll coming through. I think my next batch will be with a purer alochol solvent, this time I just used off the shelf 45% vodka, but I'll upgrade it for the next batch.

The other super cool part was inducing a vacuum on the system and watching the wash boil at 40*C, then removing the vacuum and letting it settle. Science is awesome!

[Avo]

I'm seriously just about to order some seperate Soxhlet parts, so I can participate in this fascinating part of the hobby. I'm looking at the rounded flask rather than the flat bottomed. The former can endure more stress levels. For this type you have to use the mantle type heater.
When ordering seperates you also have to make sure that the male/female tapers on the necks will marry with each other, as they come in different sizes.. I'm going for the 500 ml version, and hope to do extractions from botanicals to use with gin experimental recipies.

I've currently researched parts, and have put a kit together for $76.96 / £63.06 (extremely cheap) which includes the mantle heater and all p&p.
I am busily researching techniques on-line & You tube. One question I am asking is, I propose to use my own ethanol and have looked for information on any dilution that is necessary; as one would to do a spirit run, say 40% abv which is considered to be safe to run, or would it be run at high abv 80% + - to get the best extraction out of semi solids/lipids - safety is the prime concern, and I would think some 'Lab safety spectacles' would be a minimum requirement.

[Bushman]

What is the main difference between a Kumagawa extractor and a Sohxlet extractor?

[Avo]

https://en.wikipedia.org/wiki/Soxhlet_e ... _extractor

[Avo]

One question I am asking is, I propose to use my own ethanol and have looked for information on any dilution that is necessary; as one would to do a spirit run, say 40% abv which is considered to be safe to run, or would it be run at high abv 80% + -

I have just seen a You Tube video, and a school Lab' demo showed the pupils using Ethanol at 96% abv so question answered

[Avo]

What is the main difference between a Kumagawa extractor and a Sohxlet extractor?

Sorry Bushman, I messed up my post - Click on the Wiki, it gives a basic answer, it has to do with the thimble which holds the solids/ingredients

[Avo]

quote=Windswept post_id=7553872 time=1549375515 user_id=72536]
Here's the new setup, I've included a temperature controller since this picture so I don't have to fiddle with the controls as much. I used peppermint for this run from leftover tea bags.

Success with the new hobby Windswept. I just recently got introduced to the 'Soxhlet' process and have ordered seperates from various sources. I'm going for the 500ml size. I decided to get the round bottom flask which endures greater stresses, and consequently have ordered an economically priced electric mantle heater. I realized then that you need to purchase a second condenser to add to the set-up, so that you can recover most of the solvent; they can be purchased very cheap on AliExpress.

I have a question: with emmersion of the flask in a sand bath, how long does it take to heat up to solvent boil? thanks.

[Windswept]

I’ve never timed it, but I’d say 15-20minutes, if that. The sand bath makes a bit of a mess, but you don’t need to worry about it boiling dry, or catching fire or anything, and it was incredibly cheap!

I also use a round bottom flask.

[Avo]

I’ve never timed it, but I’d say 15-20minutes, if that. The sand bath makes a bit of a mess, but you don’t need to worry about it boiling dry, or catching fire or anything, and it was incredibly cheap!

I also use a round bottom flask.


Time heating not bad at all. I was considering an iron pot filled with sand, but then I saw some cheap electic mantle heaters for sale, so got one of those coming.