Experiment - Ethanol humulone extraction

[IvanBrew]

@moorehops, would you expect total hop consumption to be the same for a given recipe?

Example

Let's say I have a 15 gallon recipe that calls for 1 lb of hops. To keep things simple, 20% of the hops goes in at each of 5 additions, from FWH to flameout.​

Would you recommend using this extract method on the original 1 lb of hops and then add 20% of the resulting extract at each of the 5 addition times, or would you alter the hop schedule some way (time/amount)?​

 

[moorehops]

Yep you nailed it! Although your extraction may only yield 80 percent of that pound, also because you wont be losing liquid due to absorption from hop solids, so you have to keep that in mind as well. I would say do the recipe with the extract as a substitute and then use that as a basis for your next batch, if you need to add more flavor, or if you are seeking a specific addition it can probably be timed as well.

 

[IvanBrew]

I am definitely going to have a go at this.

Two more questions:

Roughly how much 95% ethanol would you expect to use processing a pound of hops?​

How long can one store the extract? (I'm assuming airtight container in refridgerator)​

 

[moorehops]

I would suggest filling a large mason jar with hops then filling it up with ethanol.
If kept in ethanol solution it can be stored indefinitely if kept away from varying temperatures and out of light.
The extract once dried can be kept good for years in the freezer if kept airtight and out of light.

 

[moorehops]

I used a little over 3 liters to process a pound. I also reclaim my alcohol for reuse but for the average home brewer, it is simpler to just air evaporate in front of a fan. It only takes about 6-10 hours.

 

[OhSoHumuLonely]

As an organic chemist, I could rotovap the stuff and save the ethanol, but.... Unfiortunately, some nasty stuff has been through these rotovaps so it would be pretty nasty not to buy a new one, but pretty expensive to do so.

 

[moorehops]

Use a solvent like isopropyl alcohol or naptha to clean your rotovap, then run high proof grain alcohol untill it is clean. Then hit it with a mr. Clean magic eraser untill she sparkles like new.

 

[IvanBrew]

I used a little over 3 liters to process a pound. I also reclaim my alcohol for reuse but for the average home brewer, it is simpler to just air evaporate in front of a fan. It only takes about 6-10 hours.

Ouch! At the cost of 3 liters of Everclear, you'd be evaporating more cash in alcohol than you're spending on hops...

Looks like I need to do some head scratching on recovering the ethanol...

 

[moorehops]

I use a very simple pot still on the stove to distill down to 10 percent alcohol, then I have a cold trap for my vacuum which also traps the last of the residual solvent. But the average home brewer should not be too concerned with alcohol recovery since most are used to heavy losses to yield being sucked up by the sponge that is hops. Haha it took me months of researching to figure out the most efficient way to extract all the lupulin without dissolving chlorophyll. All my work has been to make this an efficient enough process that it could be utilized by brewers in my area.
Its funny reading how some people are looking for efficiency in overall cost while others clearly state that its only big beer companies that are stingy squeezing every drop out of their recipes.

 

[moorehops]

I do agree about the price though. It's about $65 with the cost of hops and alcohol to run a pound. If you don't have a solvent recovery system you'll be fronting that every time you extract. You can buy simple stills on eBay for under 200 dollars to seperate your solvent from your extract. In this way you only have about 15 percent solvent loss and your cost should drop to about 5 dollars an extraction.

 

[IvanBrew]

Its funny reading how some people are looking for efficiency in overall cost while others clearly state that its only big beer companies that are stingy squeezing every drop out of their recipes.

I'm an odd duck when it comes to spending money. I'll invest insane amounts of time into researching the best way to do something and spend freely, sometimes extravagantly, on equipment and process. At the same time, I'm a Scrooge on batch costs. A lot of that research and spending goes into getting my per batch costs down, i.e. improving efficiency, yeast banking, etc...

I didn't think a pot still could hit 95%. Wouldn't you need a reflux tower to get back to the original solvent concentration?

 

[moorehops]

I pack the column tight with mesh and it increases the surface area. Once it has built up enough to hit my water jacketed condenser, it pours out of my still like a sweet solvent fountain! If you dont get a high enough proof, simply distill it again.

 

[moorehops]

Plus since this is simply solvent recovery and you aren't distilling a wash. Recovery should only take about an hour. Just make sure you leave at least 10 percent volume so you can pour your extract into a dish to dry, If you boil it dry you will have a Heck of a time cleaning out your still.

If you get a still then this process is pretty efficient and when it comes to final yields it is superior, you wont lose 20-40 percent that is normally soaked up by hops. Utilizing the flavor compounds and aromas of different strains you canend up with precisely the hop flavor you are aiming for.

 

[IvanBrew]

I will be trying this on the next batch of my house pale. If I like the results, I see a still in my future...

Thanks again for all the info and insight on this!

 

[OhSoHumuLonely]

Let us know your results! Maybe these extracts will become the standard. Thinking outside the pellet.

Sent from my PantechP8010 using Home Brew mobile app

 

[moorehops]

Just finished extracting some chinook hops! Talk about a blast of spicy pine!
I believe there will be a new wave of craft extracts of all kinds soon.

 

[OhSoHumuLonely]

Man, I bet citra would smell good!

How much do I gotta pay you to ship me a test batch of this stuff?

Sent from my PantechP8010 using Home Brew mobile app

 

[moorehops]

why dont you message me your email or number and I'll get in touch for samples?
Citra hops would be great but ive yet to get them, they are often the first hops sold out. So far ive only processed cadcade, chinook and crystal hops. All 3 extracts have had identical aromas to the strains they were extracted from.
Crystal hops were a medium yellow lupulin, floral with a grassy, lemon hop aroma.
Cascade was very bitter citrus, almost like an orange peel.
Chinook was like a spicy pine forest with grapefruit aroma

 

[OhSoHumuLonely]

Done.

Sent from my PantechP8010 using Home Brew mobile app

 

[Adam_Selene]

Further refining with my vacuum doesnt cause oxidation...where is the oxygen in a vacuum It is a perfectly workable product as is. You stir it into the boil. What is soluble is the same as when you use whole hops, only with the extract you dont lose any of your yield due to absorption. It can also be used to dry hop or to resinate a bottle for the beer to age in.
The nonpolar gas is not something crazy no. Its soluble in lipids/fats/oils and it dissolves into ethanol to form a better solvent. It is purged entirely once it is released to normal atmospheric pressure. The reason I dont release details is because no one has figured this out but me and its very clear in my reasearch. Its not complicated, however I plan on selling my extracts and I worked very hard figuring out the trial and error to make an efficient useable product.

... Nitrogen??

 

[moorehops]

Close with nitrogen, but still nope. Sorry, that one is a trade secret
It allows me to harvest all the Lupulin in just under 2 minutes. While only using ethanol extracts roughly 75-80 percent.
I gave everyone a huge leg up on understanding what you want to extract. Even on professional brewing websites ethanol extract is listed as " a dark green, viscous paste." If that is the alternative, choose real hops everytime...however now you know that is not what you want, you can move on to smarter, tastier brewing.
The reason it is green is because they are simply dissolving the entire hop into ethanol. This means chlorophyll, plant waxes and other gross solubles have been extracted as well.
Look at the strain to tell what color the lupulin will be.
The color of chinook lupulin is dark yellow, I know ive extracted correctly when it is exactly the color of strains lupulin glands.

 

[Adam_Selene]

Close with nitrogen, but still nope. Sorry, that one is a trade secret

... ARGON??

It allows me to harvest all the Lupulin in just under 2 minutes. While only using ethanol extracts roughly 75-80 percent.
I gave everyone a huge leg up on understanding what you want to extract. Even on professional brewing websites ethanol extract is listed as " a dark green, viscous paste." If that is the alternative, choose real hops everytime...however now you know that is not what you want, you can move on to smarter, tastier brewing.
The reason it is green is because they are simply dissolving the entire hop into ethanol. This means chlorophyll, plant waxes and other gross solubles have been extracted as well.
Look at the strain to tell what color the lupulin will be.
The color of chinook lupulin is dark yellow, I know ive extracted correctly when it is exactly the color of strains lupulin glands.

It's not Co2 right? Your not dropping dry ice in one end and somehow condensing the product on the other end? I know that your not going to tell me, but... is that something that you have tried? =D

 

[moorehops]

No, but the industry uses liquid co2 and supercritical co2 to make extracts. They are actually very cheaply priced because the extraction machine recycles 97 percent of the co2 used. While co2 extracts are high quality, they are typically made from generic hops and wont have any strain specific flavors or aromas.
The machines to extract using co2 are also incredibly expensive, almost 10 times more expensive then all your home brew equipment combined.

 

[moorehops]

I believe argon dissolves into water, not ethanol...but dont quote me on that.
Although I believe argon to be too inert to aid in extraction, you could very much store your extract under an argon atmosphere to prevent oxidation. But I havent even taken storage that far. Ive found a cobalt blue or brown glass sealed airtight is perfectly acceptable for years of storage.

 

[ColumbusAmongus]

That's what I meant. Sorry, lower pH (raises [H+]) in order to not extract tannins and the like.

Acid conditions will also favor isomerization I believe.

Not sure if I ever mentioned this but there is a paper by Horst Koller (1968) that looked at more efficient isomerization in a magnesium chloride solution. I think you could easily adapt it to food safe stuff (using vodka instead of water / methanol), skipping the pH adjustments and extractions, and using CaCl2 instead of MgCl2.

They used 15mmoles (3 grams) of MgCl2 dissolved in 50ml of water and 70ml of methanol. Heated to 70C for 10 minutes under nitrogen kept at pH 7.2-7.5 with NaOH. They acidified and extracted with solvents to recover their IAA.

Lets say you used vodka because methanol is a bad idea. I don't like the high amounts of magnesium also…it seems like 3 grams would be a lot to add to your batch of beer. They mention Ca++ and Mn++ should work as well so CaCl2 might be a good substitution since it is a common brewing salt.

**Edit - forgot to mention…the paper cites that the added cations increase the isomerization rate by 200 fold.

If you were to heat up some vodka and if the CaCl2 actually dissolves in the mix, you could steep hops in the mix like a tea and in 10-20 minutes have a high IBU tea to add to your beer. Meyah? You wouldn't need to extract, just dump the vodka tea into your beer. I am thinking that the lower temps would help prevent your oils from driving off and the quick isomeriztion would help you solubilize more IAA before they drive off.

Who is going to try it?

 

[fearwig]

Shouldn't the holy grail of hop extraction be aromatic additions, not bittering? I mean the cost of bittering hops is such that "efficient isomerization" is a phrase that should only be said by BMC-scale (and probably quailty) brewers, don't you think?

Not to rain on the mad science parade, I wholly support a futile end if the means to accomplish it is sufficiently insane.

 

[helibrewer]

Shouldn't the holy grail of hop extraction be aromatic additions, not bittering? I mean the cost of bittering hops is such that "efficient isomerization" is a phrase that should only be said by BMC-scale (and probably quailty) brewers, don't you think?

Not to rain on the mad science parade, I wholly support a futile end if the means to accomplish it is sufficiently insane.

I believe part of the OP's point was the reduction of losses (increasing brewhouse efficiency) by eliminating the liquid absorbed by all the hop matter...greatly reducing trub. Also, all those bittering hops are contributing a lot of plant matter flavors you might want to eliminate.

 

[fearwig]

Not to derail this thread (it's awesomely informative, especially the "3 minutes" rule and freezing of hops for ethanol extraction), but I decant my trub into a 1-gallon carboy (squeezing it out and briefly repasteurizing before crashing, if leaf) and let it settle in the fridge for a day or two after the boil, then add to active fermentation or save it for a starter. Works like a charm, no waste, no trub in your primary, and you gain half a gallon of wort on most boils. Now someone may say, "That's a lot of work, to hell with that!", but if you're otherwise thinking about dissolving alpha acids in argon under pressure with a flux capacitor...

I get how you might want to minimize certain planty flavors in a big DIPA or something, though. I still think this is a great thread, but only because I want to dissolve those aromatic compounds into a solution so I can get an "instant dry hop" I can fine-tune. I'm strongly considering stockpiling grain alcohol to experiment with, since it sounds like Maryland is in the process of illegalizing it (!).

 

[moorehops]

Lol dissolving under argon and a flux capacitor
Thats about the guess everyone has given me lol. The nonpolar gas is not critical to the extraction, ive simply tweaked my method to operate at maximum efficiency.

However, it doesnt need to be complicated. Extracting hops strain specific lupulin from the hops is simple with grain alcohol. 5 minutes is almost too long, 20 minutes and it'll be green. If you leave it for days or weeks itll dissolve into a nasty green mixture, if you boil it in a soxhlet extractor you will dissolve it into green pasty waste.

The lupulin glands hold the alpha, beta acids and the essential oils. If you extract all the lupulin in a 3 minute wash, you now have all the alpha, beta, and essential oils used for the flavoring and aromatics of your beer. If added to the beginning it will isomerize like normal hops, if left untill later it will not isomerize and it will retain the the volatile aromatics.

 

[Wynne-R]

No worries, fearwig, vodka will do. The only reason I used everclear is that it was slightly less expensive. I also thought it might be better than the cheap vodka in plastic jugs.

Any idea what the flux capacitor would do with tachyons?

My extractions might be a little green, mostly amber and cloudy. I’ll try to remember to take a picture next time.