Steam Distillation of Hops

[kevink]

Sorry, didn't see that. Can you fluff it up with some rice hulls? I'm kind of serious.

 

[passedpawn]

Sorry, didn't see that. Can you fluff it up with some rice hulls? I'm kind of serious.

Great idea - didn't occur to me. I don't use them in my brewing (system is mostly stuck-proof). I'll pick some up and try the pellets again. Think the hulls contain any oils?

 

[fragged]

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.

 

[ancientmariner52]

You could try distilling rice hulls alone and see if anything nasty turns up.

 

[KLITE]

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?

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!

 

[passedpawn]

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!

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]

next thing = rotary evaporator????

 

[passedpawn]

next thing = rotary evaporator????

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).

 

[clearwaterbrewer]

I might get one for myself as a present... will let you play on it as long as what you put in it is legal ;-)

 

[passedpawn]

I might get one for myself as a present... will let you play on it as long as what you put in it is legal ;-)

Yes!

 

[RoadKing]

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.

Please be careful, with that top chamber clogged, the steam in the boiler has no where to go an could explode! I would at least try to get some sort of screen, or even a stainless scrubby at the inlet of the top chamber to keep it from clogging and allow vapor to pass through unimpeded.

 

[passedpawn]

Please be careful, with that top chamber clogged, the steam in the boiler has no where to go an could explode! I would at least try to get some sort of screen, or even a stainless scrubby at the inlet of the top chamber to keep it from clogging and allow vapor to pass through unimpeded.

Thanks for the concern. I do have a metal screen in the neck there between the biomass flask and the boil flask. That should help.

 

[passedpawn]

I found some sort of hairy needled shrub at the local park yesterday and brought home some branches. It's some sort of conifer with the long needles and cones. The needles smell very strongly of lemon and pine.

Stuffed the biomass flask full of those needles and got some oil. Getting it going again right now.

I've got some rice hulls here, so I might take another shot at extracting from pellets.

 

[passedpawn]

Getting oil from the pine needles now.

 

[clearwaterbrewer]

This was just purchased and is on it's way... obviously I will need a larger flask, but this is the mac-daddy Buchi R-215... with vacuum controller.. I need to get my small chiller set up and see if my automotive vacuum pump is good enough or if I need to get a buchi one... here is a link to a video also:

 

[passedpawn]

This was just purchased and is on it's way... obviously I will need a larger flask, but this is the mac-daddy Buchi R-215... with vacuum controller.. I need to get my small chiller set up and see if my automotive vacuum pump is good enough or if I need to get a buchi one... here is a link to a video also

When can I come by and see it

 

[clearwaterbrewer]

soon, it just arrived!

 

[Shine0n]

Distilling high abv alcohol is a no no, lower the % below 30% as it will gain abv by the distillation process.
Also, the hops not letting the flow through could pose a problem, BOOM!
Pressure could build and I for one wouldn't want that to happen during the run or for anyone to get hurt expecially with boiling fluids and shards of glass flying about.
Keep a loose packed section and something that won't pack down once wet.

 

[passedpawn]

I added one drop of this stuff to a glass of pale ale last night. Ruined it. Very strong hop aroma, but not in a good way, harsh, solventy, not the aroma you want. I thought it'd kill the head, but oddly I think it improved it. The head on that glass of homebrew never went away.

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.

 

[clearwaterbrewer]

I wonder if the isomerization is happening in the extraction process and the hydrosol or oil can be dosed into beers... dosing anything smaller than a keg will be painstaking, but might be worth it..

 

[passedpawn]

I wonder if the isomerization is happening in the extraction process and the hydrosol or oil can be dosed into beers... dosing anything smaller than a keg will be painstaking, but might be worth it..

I could try that. I did save it for that purpose. I'll comment later when I do it.

 

[lump42]

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?

Are you sure the alpha acids are evaporating into the steam at all? Humulone boiling temp is 571.4±50.0 °C (1060.5 ± 122 °F) (source). I couldn't find a boiling temp for isohumulone. You might just try making a small batch and use the spent hop as bittering. See if it does the trick.

 

[passedpawn]

Are you sure the alpha acids are evaporating into the steam at all? Humulone boiling temp is 571.4±50.0 °C (1060.5 ± 122 °F) (source). I couldn't find a boiling temp for isohumulone. You might just try making a small batch and use the spent hop as bittering. See if it does the trick.

Hmmm. I froze the spent hops, so I could try that. I rarely do a "small" batch though Maybe I'll pick up some DME and do a 1g test this weekend.

 

[GrandwizzardGillias]

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.

I bought a soxhlet on e bay if you use a mesh bag or filter bag in place of the thimble there is plenty of room for the hopps

 

[fragged]

This was just purchased and is on it's way... obviously I will need a larger flask, but this is the mac-daddy Buchi R-215... with vacuum controller.. I need to get my small chiller set up and see if my automotive vacuum pump is good enough or if I need to get a buchi one... here is a link to a video also:

So jealous, so many other fun experiments you can do with this.

Your auto pump shouldn't be an issue, just be sure to have a way to regulate the vacuum (a tee in the vaccum supply line with a valve going to atmosphere should work).

The following assumes tou are using alcohol in the extraction: Simply because I'm a little over cautious, I'd also put a condenser in that same line just to be sure I didn't pull any alcohol vapor into the pump. Given the temps, I doubt it would condense in the pump (contaminating the oil). However, I still wouldn't be hot on possibly pulling highly explosive vapor into atmosphere, especially indoors.

Finally, I'd also put a one way valve on the pump vacuum supply(assuming the apparatus doesn't come with one). This will keep the system from pulling all the oil from the pump into the system when you inevitably forget to shut the pump off without closing the supply valve. With that said, a check valve installed where I mentioned would eliminate the need to have a valve in the supply line, outside of the bleed off valve I mentioned.

 

[DemonsRun]

I added one drop of this stuff to a glass of pale ale last night. Ruined it....

I have some samples of Hopzoil from Glacier farms (Chinook & El Dorado), at CBC to sample they just stuck the tip of a toothpick in then swirled the toothpick in your beer and that was strong. I dosed 4 gallons of an IPA with .25ml of the El Dorado and it took over a month to calm down to a drinkable level. Wasn't solventy but it did seem to be missing some balance that I would get if I had used pellets to dry-hop. However I could see using just a bit to kick up the aroma (a very very tiny bit).

Also the tetrahydro-iso-alpha-acids in hops greatly improve head re-tention, Hopsteiner sells an extract of just these acids which apparently add some bitterness as well.
https://www.hopsteiner.com/wp-content/uploads/2017/11/13_09_Tetra.pdf

 

[ain]

Great topic. Subscribed.

 

[corkybstewart]

Have you tried with fresh hops?

 

[passedpawn]

Have you tried with fresh hops?

Sorry, guess I missed this. No, I have not gone back to hops yet. In fact I didn't use the ones I extracted... I chickened out.

I did attempt to extract oils from gardenia, but that produced exactly NOTHING. Dang it.

I'll be setting it back up in the next couple of weeks to extract more pine essential oil. That worked out really well.

 

[Jayjay1976]

Sorry, guess I missed this. No, I have not gone back to hops yet. In fact I didn't use the ones I extracted... I chickened out.

I did attempt to extract oils from gardenia, but that produced exactly NOTHING. Dang it.

I'll be setting it back up in the next couple of weeks to extract more pine essential oil. That worked out really well.

Brewing aside, do you think a hop-flavored bitter, for mixing cocktails, makes any sense?