Steam Distillation of Hops

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passedpawn

passedpawn

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I figured the distilling forum was as good a place as any for this. I got this toy for making essential oils from various stuff. Today, hops. Still in the process. Biomass flask contains 4 oz of citra.

I'm not sure how to use the oil. In fact, I'm not fully sure what I'm doing here. But having fun anyway.

What's going on?
  • boil flask (RODI water) creates steam
  • steam rises through the biomass flask (hops here)
  • steam enters the still head where it starts to condense; note it's slanted slightly downward
  • graham condenser completes the condensing of the steam to liquid; the condensed steam drips down that curly glass tubing in the middle. Chlled water is passing around it, from bottom to top (see rubber tubing to small submersible fountain pump in HD bucket). It's basically a counterflow chiller.
  • separatory trap captures the oil, floating on top of water. See second picture, yellow hop oil floating on column of water. It's designed so that if it fills, the water will overflow out the side tube and you don't lose any oil. The stopcock allows you, in the end, to drain the water, then drain the oil into a vial.

full


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And they said you were mad! Mad!

Passedpawn, you are having way too much fun.

Stealth, the valve on the end of a railcar, that's called an angle cock. Go on, laugh and get it over with. [emoji16]
 
I'm guessing it takes a ton of hops to make a little essential oil?

I know in a pot still starting with 4 gallons of wash ended up in about 1 cup of whiskey.

Coming from such a frugal background, it seems like a waste in some ways.
 
Yooper said:
I'm guessing it takes a ton of hops to make a little essential oil?

I know in a pot still starting with 4 gallons of wash ended up in about 1 cup of whiskey.

Coming from such a frugal background, it seems like a waste in some ways.
Click to expand...

Nothing wasted really (at least not yet). The output from this process is
  • hop oil
  • hydrosol (water that's gone through the process, smells wonderfully like hops)
  • wet hops
I'm planning an all-citra IPL brewing session monday. I'm gonna try to use all of this. Not sure exactly how yet, but I don't intend on wasting anything. I can't exactly say what the benefit of this experiment was, but I'm hoping I can reduce the hop trub in the bottom of my fermentor. Man, I must have 3 or 4 inches when I finish a hoppy IPA.

This is all just practice for when my gardenia and magnolia bloom. I've been wanting to capture their oils for years after watching their sadly short, but intensily aromatic, blossoming time. We like to burn essential oils around the house.
 
I like essential oils too, and grow my own rosemary and lavender, and the lilacs are awesome. I'd even like to get some echinacea essential oil, to have for cold and flu season.

Please let me know how much you get out vs the amount of flowers you need. I'd really like to get into this!

Can you tell me more about the set up? I'd like something that doesn't take up a ton of room, or cost a small fortune!
 
Yooper said:
I like essential oils too, and grow my own rosemary and lavender, and the lilacs are awesome. I'd even like to get some echinacea essential oil, to have for cold and flu season.

Please let me know how much you get out vs the amount of flowers you need. I'd really like to get into this!

Can you tell me more about the set up? I'd like something that doesn't take up a ton of room, or cost a small fortune!
Click to expand...

It doesn't take too much space. As you can see above, the assembly doesn't take up much real estate when set up. It all breaks down into a single box which is nice. Cost is a bit prohibitive though. This setup I have here is about $300.
 
The distillate is:
  1. hydrosol, which is the aqueous part, and VERY aromatic. It's on the bottom of the separator picture above.
  2. hop oil.

I just measured the pH of the hydrosol and it's 5.4. It started out as RODI, presumably very close to 7. So there's some acid in there. Also, the boil flask is now a dark color. During the boil, stuff does drip back down in there. I wonder what amount of hop acids and oils are in there?
 
Very cool setup. I don’t see a need for a large motor to make that work, but if you did need one the wiring box connected to the motor would be called a “peckerhead”.
 
Yooper said:
Very interesting! What is your plan for the hydrosol?
Click to expand...

ah heck, I haven't formulated a plan. I did some online research and wasn't very successful.

I'm trying to figure out:
  • where the bittering acids go, whether into the oil phase or the aqueous (hydrosol). I need those acids for bittering.
  • bittering addition: do I need to boil at all? In theory, I should have full isomerization now, so can I just add after boil? How much of that?
  • which part is gonna give me going to replace dry hopping? How much of that?
  • Is there any use for theses spent hop leafs? I saved them, but in theory they should be fully spent. Does steam really strip them completely?
 
passedpawn said:
Some of them must be handled with care. I've been reading on some essential oil sites of hazards. I think it's mainly due to the concentration, and not a chemical change to the substance, but I'm not positive.
Click to expand...
Seems you are in uncharted territory, you could be the first person to explore the side effects of hop overdose!
 
Testing extraction from pellets. This is 5 oz of 6.9% AA Jester hops. Not getting too much. Probably has something to do with how well the steam can saturate and escape the biomass. There's not good way to "stir them up". Might be better to just boil them in the boil flask, might try that after a while.

full
 
passedpawn said:
Some of them must be handled with care. I've been reading on some essential oil sites of hazards. I think it's mainly due to the concentration, and not a chemical change to the substance, but I'm not positive.
Click to expand...

It was the concentration I was referring to. I did not think that this process - and your set up looks really incredible - produces any hazardous new compounds. But the concentrations of the volatile substances are very high. I see that they are sometimes used in food but most often I think they are used aromatically.
 
I'm thinking I shouldn't be on this thread at work. Lack of productivity aside, the wrong person walks passed my computer with one of those pictures up, I'm bound to be meeting with HR in the next couple days lol.

Joking aside, this looks really interesting. Does the oil retain the aroma of the hops? Could it be used in a diffuser to make a room smell delicious? Or am I thinking of a different kind of oil?
 
WFox93 said:
I'm thinking I shouldn't be on this thread at work. Lack of productivity aside, the wrong person walks passed my computer with one of those pictures up, I'm bound to be meeting with HR in the next couple days lol.

Joking aside, this looks really interesting. Does the oil retain the aroma of the hops? Could it be used in a diffuser to make a room smell delicious? Or am I thinking of a different kind of oil?
Click to expand...

Oh yea, the oil is extremely aromatic. I'm still not sure what to do with it though.
 
I would use it as a dry hop. This is very similar to hopzoil (though they use fresh hops to distill if I remember correctly) and that's the recommended use. So yeah, rack to keg, toss it in and see what youget!
 
passedpawn said:
From 5 oz of that hop above I got 2.2g of oil extract. I saved the leaf hops into vacuum bags for a brew later. Also saved the hydrosol, 2 pints.

full
Click to expand...

How does that compare to the advertised total oil content of Citra? I am too lazy to do the math.
 
kevink said:
How does that compare to the advertised total oil content of Citra? I am too lazy to do the math.
Click to expand...

Well, let's see:

Grams of Citra that I used: 142g (5 ounces)
Grams of oil that I extracted: 2.5g
Theoretical Oil Content (from online stats): 3.55g (142g * (2.5mL / 100g)
Calculated efficiency: 70% (3.5g/3.55g * 100%)

So, I'm pretty happy. Sources of loss:
  • There was certainly oils left clinging to the condenser, and especially the still head. I can still see a lot of droplets in there when done, and I believe they are oil. I could have used some sort of solvent in there to rinse, then gone through a bunch of effort to remove that solvent, but I'm no chemist.
  • I believe that packing the biomass with less stuff makes it more efficient. I actually extracted from 4oz of hops first, then an additional 1oz in a second batch. I believe the latter produced almost half as much as the first batch.
  • Though the condenser seems to work really well, it's possible that some steam still exited the system carrying oil.
  • I'm using the numbers from the online stats. I have no idea if 2.2mL/100g or 2.8mL/100g is the correct number for my hops. Pictured below is the only info I have for the actual hops I used.

upload_2017-12-14_12-39-0.png

upload_2017-12-14_12-52-28.png
 
Not bad at all! I usually assume my hops are right in the middle of the range. Should be close enough! When are you going to try pellets?!
 
kevink said:
Not bad at all! I usually assume my hops are right in the middle of the range. Should be close enough! When are you going to try pellets?!
Click to expand...

I did. Didn't work well at all. Got very little - essential a failed experiment. Post #19 is what it looked like as the pellets swelled. The steam had a hard time getting through the pellet mash. I could see a lot of condensation falling back into the boil flask.
 
Sorry, didn't see that. Can you fluff it up with some rice hulls? I'm kind of serious.
 
I'd guess that using an ethanol wash in an erlemeyer first, then filtering the debris off, then distilling most of the ethanol back out would result in a more thorough oil collection. If you do it now, you'll probably clean that residue from your condenser as well from the ethanol vapor, giving you more to redestill to get all that's possible.

Use everclear, if they have it where you live. The lower the proof, the higher the temp you'll need, though I'd guess you'll get most of the alcohol out between 170 and 200.

Bear in mind, if not sealed, you may get some alcohol vapor during the distilling, so vent accordingly.


I may try this with the pound of citra that was rotten when I got it a couple days ago. Theoretically, I should be able to leave the dead bacteria that made them brown behind. May need to add a freeze step for that.
 
passedpawn said:
ah heck, I haven't formulated a plan. I did some online research and wasn't very successful.

I'm trying to figure out:
  • where the bittering acids go, whether into the oil phase or the aqueous (hydrosol). I need those acids for bittering.
  • bittering addition: do I need to boil at all? In theory, I should have full isomerization now, so can I just add after boil? How much of that?
  • which part is gonna give me going to replace dry hopping? How much of that?
  • Is there any use for theses spent hop leafs? I saved them, but in theory they should be fully spent. Does steam really strip them completely?
Click to expand...

Not a bad set up my friend! I for one dont like steam as a form of distillation because steam can volatilize and decarboxylize some of the more interesting compounds due to its higher temperature.

Im curious how does it smell? does it smell better than the hops? If so then your method might be working well.

As to your question the acids need to be izomerized and that can only be done through temperature, i doubt the hydrosol solution would have a useable amount of acids, i bet theyre still in the hops. You can most certainly reuse those hops for bittering additions but im sure that if there are any essnetial oils left their amount is negligible . Sounds like a decent return about 1.8/2 ml per 100gr is sort of the amount that the hops can have.

My advice is collect about 20/30 ml of that oil mix with a tiny bit of alcohol just so it mixes and into a keg it a goes.

Since you seem a interested in this type of stuff try a soxhlet extraction with everclear (heck even distill your own). Do it at minus 20C with whole flower hops, **** pellets man. and once done get some activated carbon filter to get rid of the chlorophyl, do a little vacuum purge at cold temp just to boil some of the alcohol off and tadam better than any co2 extract anyone will sell you.

Good luck!
 
KLITE said:
Not a bad set up my friend! I for one dont like steam as a form of distillation because steam can volatilize and decarboxylize some of the more interesting compounds due to its higher temperature.

Im curious how does it smell? does it smell better than the hops? If so then your method might be working well.

As to your question the acids need to be izomerized and that can only be done through temperature, i doubt the hydrosol solution would have a useable amount of acids, i bet theyre still in the hops. You can most certainly reuse those hops for bittering additions but im sure that if there are any essnetial oils left their amount is negligible . Sounds like a decent return about 1.8/2 ml per 100gr is sort of the amount that the hops can have.

My advice is collect about 20/30 ml of that oil mix with a tiny bit of alcohol just so it mixes and into a keg it a goes.

Since you seem a interested in this type of stuff try a soxhlet extraction with everclear (heck even distill your own). Do it at minus 20C with whole flower hops, fudge pellets man. and once done get some activated carbon filter to get rid of the chlorophyl, do a little vacuum purge at cold temp just to boil some of the alcohol off and tadam better than any co2 extract anyone will sell you.

Good luck!
Click to expand...


Yea, I've been looking at a soxhlet extractors for a while on ebay. I think I'd need a different condenser to make that work correctly though (alihn). Glassware on ebay is pretty cheap, no reason not to try it. Soxhlets look pretty small though, don't think leaf hops would work well there.

Thanks for the comments. I'm interested a lot. We'll see how long before I move on to the next thing though.
 
clearwaterbrewer said:
next thing = rotary evaporator????
Click to expand...

I looked at them, with vacuum. Very cool. I think the same can be done by waiting? I saw a lot of videos of chemists drying the water part of immiscible mixtures using them. Cheapest on ebay was still fairly expensive. IBU assay is much more achievable right now, and that's kinda what I want to play with. Chemicals can be a bit pricey, but you can find centrifuges very cheap, even on amazon, and that's the only necessary equipment (need a way to do UV absorption measurements, but I've got that covered).
 

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