Experiment - Ethanol humulone extraction

[masonsjax]

I do extractions of hop strains using ethanol and a nonpolar inert gas under a pressurized atmosphere to yield a beautiful hop extract used at the end of boiling.

Does this process require expensive specialized equipment or is it feasible for your average homebrewer to pull it off themselves? Could you elaborate a little on what the process involves if it is something we might be capable of doing at home? Thanks.

 

[moorehops]

yes it does require special equipment, but it isnt expensive. the extraction process ive been using is unique and of my own design, Id love to go into details but I've spent the last 4 months perfecting the process.
I will however disclose the essentials behind a very easy home extraction!
It is not as efficient as my method, but it is very close and will still provide a phenomenal extract.
First you need 190 everclear alcohol or 151 proof. The higher the proof the better, stick with drinking alcohol to keep food quality. I stick the ethanol in the freezer into an salted ice bath to get the temperature well below freezing. The hops I'm extractimg from are also kept in the freezer. Freezing the hops ties up the chlorophyll and the other water solubles.
Next the two are mixed into a mason jar and shaken hard for 1-2 minutes and returned to the freezer for the next two minutes. Remove from freezer, shake the mix hard one last time then strain through a coffee filter into a baking dish.
Let the baking dish sit out and the alcohol will evaporate leaving behind your hop extract. Scrape with a razor blade and collect on to silicon sheet or parchment paper.

 

[moorehops]

Here are pictures of the extraction, what it looks like as its evaporating and the final product.

 

[moorehops]

if your extract has turned green you've left it in the alcohol too long and its extracting chloryphyll and plant waxes. If kept under 3 minutes total contact time with frozen material, The extract should be anywhere from bright yellow to a warm amber. You will have extracted 70-80 percent of the lupulin glands free of any chlorophyll and non aromatic plant waxes.

 

[OhSoHumuLonely]

You are serious, man! By the way, welcome to the forums.

 

[mchrispen]

From the pictures, you are using whole hops. How well does this work with pellet?

 

[moorehops]

Thanks! Ive never used pellets as my normal extraction using my non polar gas is much more efficient with whole hops. Although I imagine it would work fine if subtituted for whole leaf. Although filtering may be a bummer if the pellets turn to mush.

 

[AlCophile]

I use 70% EtOH, as can no longer buy grain alcohol here. I originally used it to increase the "hoppiness" of commercial beers, but found it works reasonably well with homebrews which turned out to be underhopped. One problem is that once the extract hits water(beer), some organics precipitate out. If you try this with plain water, you will get an off-white powder, which I cannot analyze. It may be instructive to boil that powder at pH 5 or so.

 

[masonsjax]

Moorehops, thanks for the detailed write up! I'm going to give this a whirl.

 

[moorehops]

Do you mean 70 proof or 70 percent alcohol. Cause I use 151 proof which is 75 percent alcohol when I've run out of 190 proof and I dont get a white powder...do you evaporate all the alcohol? Or are you just adding oil/alcohol into the beer. If you are your talking about the ouzo effect, when alcohol is mixed with water and it produces a milky white cloudy effect. google ouzo effect.
In order to produce a pure extract you need to evaporate all the alcohol and water. It works faster with high proof, but if you set it in front of a fan in a baking dish where it will be a thin film it will evaporate.

 

[moorehops]

Moorehops, thanks for the detailed write up! I'm going to give this a whirl.

Thanks masonsjax! If you have any further questions send me a message and I'll give you my email address.
Ps I suggest freezing your hops in the mason jar you'll be extracting in. Also remember short contact time. Most definitely under 5 minutes, Best done with 3 minutes. Be patient with the drying process. Use a razor blade to scrape the resin from your dish. Enjoy the smell! It'll male your house smell just like the strain your extracting from.

 

[moorehops]

Further refining can be done by removing the non aromatic waxes by re dissolving your extract into warm ethanol, then freezing it. Once it is below freezing you need to filter it through a coffee filter while keeping it in the freezer. Once it is done filtering pour your alcohol mix back in your baking dish in front of a fan to evaporate. I further refine my extract by purging in a vacuum chamber. This now pure hop absolute can be added directly to your beer. I like the idea of a resinated bottle to age beer in
Cheers

 

[fearwig]

Nobody’s mentioned pH. I’m no chemist, but here’s what I have come up with experimentally as a dryhop substitute:

I like this! Can you ballpark your target pH so I can use citric? pH5ish?

Moorehops: Your method is interesting too, but why do you want to make hop hash? Isn't it more useful in solution?!

 

[moorehops]

No way. You extract everything you want from the hops without sacrificing brew yield, plus you end up with a much cleaner taste avoiding the water solubles and chlorophyll that end up in your brew when you use whole hops or pellets. Not to mention you can use the extract at anytime during the boil or while hot. Seems like the superior method, especially when dry hopping is concerned considering no yield will be lost.

 

[moorehops]

Hop hash. Hilarious! Yes my method could technically extract from any other herb or fruit. But the most ive experimented with was cocoa from cocoa nibs and strawberry resin which both were added to bottled beer. So delightful! But thats when I was getting all mad science when I finished testing my chamber.

 

[fearwig]

Well, you're going to have to dissolve it in something, and since what you're trying to add is aroma, presumably it's post-primary wort--that's what I'd use it for, anyway. So I think a super-concentrated solution would be more useful than a resin/solid for that purpose, because you have to redissolve it. I think my ideal medium would be something like 10-50ml of ethanol per 5gal batch, a drop in the bucket so to speak.

Not really a criticism of your method, except for that practical aspect and the fact that each additional evaporation presumably oxidizes some desirable compounds (maybe not enough to matter).

 

[Wynne-R]

Fearwig, a couple of datapoints.

I just added .5 ml of 85% phosphoric to 500mL of tapwater and it came out pH 2.0. Interestingly, the mix of acid, water, alcohol and hops combined with 250 mL of additional water and 100g priming sugar is 5.4

As my old boss used to say, I don’t understand all I know about this.

 

[OhSoHumuLonely]

This "nonpolar gas" -- is it a proprietary gas o' somein? It's not like 1,1,2-trifluoroethane or something crazy, is it?

Sent from my PantechP8010 using Home Brew mobile app

 

[fearwig]

Fearwig, a couple of datapoints.

I just added .5 ml of 85% phosphoric to 500mL of tapwater and it came out pH 2.0. Interestingly, the mix of acid, water, alcohol and hops combined with 250 mL of additional water and 100g priming sugar is 5.4

As my old boss used to say, I don’t understand all I know about this.

Earlier I was thinking, "Why am I asking him, when I could just titrate that? And first learn how to do said titration because I failed AP Chem a decade ago?" Glad I asked.

 

[moorehops]

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.

 

[moorehops]

Well, you're going to have to dissolve it in something, and since what you're trying to add is aroma, presumably it's post-primary wort--that's what I'd use it for, anyway. So I think a super-concentrated solution would be more useful than a resin/solid for that purpose, because you have to redissolve it. I think my ideal medium would be something like 10-50ml of ethanol per 5gal batch, a drop in the bucket so to speak.

Not really a criticism of your method, except for that practical aspect and the fact that each additional evaporation presumably oxidizes some desirable compounds (maybe not enough to matter).

Well no, you would dissolve it in beer. If you dissolve it into a solution of ethanol first, the instant you dump it into the beer you will get a milky white cloud called the ouzo effect. The oil will then float to the top, pool, and all the volatile aromatics will boil off first.
Alternatively, you could add the extract directly to the boil and let it dissolve as hops normally behave. Slowly and throughout the boil.

 

[moorehops]

And once again dry hopping with extract is easy, only a certain percentage of oil is soluble in the alcohol in beer. You could run a test with plain alcohol cut with water to the percentage of your beer, say 10 percent. See how much extract will dissolve in 10 percent. Now you know pretty accurately the ratio of oil to beer and you can cut down on waste.
Regardless of when the extract is used, the idea is you are removing the diluted plant waste that yields yuck tastes and in turn that frees up the solubility of the beer for all the tasty oils!

 

[fearwig]

Yeah, post-primary beer I meant, not wort.

So solubility of these solids is sufficient that you can use in the bottle without someone eating a hop nugget? Because I am thinking of these applications for postboil, myself.

Liquids are also easier for a user to measure, of course. I get what you're saying about the oils separating when you add it to beer from the ethanol extract, but then getting the extract into a roughly beer-like concentration of alcohol for delivery seems like a good alternative, even if you have to add 250ml to your beer or more... I dunno the delivery of a solid extract is hard for me to wrap my head around.

 

[moorehops]

Yes, if you have filtered the extract before evaporation your oil will dissolve into the beer up to a point. Obviously a gram which is almost the equivalent of a quarter pound of hops, isnt going to taste great in a pint, But a 100th of a gram might be what you are looking for.

 

[moorehops]

Experiment! Have fun! I've given everyone a huge headstart on extracts. The common idea everyone keeps posting is steeping hops in alcohol for days to weeks, every website that describes ethanol hop extract as a thick dark green viscous paste. These extracts are very SUB PAR, they are diluted with tons of plant wax, chlorophyll and glandular material.
The REAL QUALITY extraction needs to be very quick, 3 minutes-5minutes.
It should be the color of the lupulin you are extracting. Light yellow to dark yellow to amber. The flavor difference is incredible and it is very possible for every homebrewer to use it. Just need your hop strain, high proof grain alcohol, a mason jar, coffee filters and a glass baking dish. Extractions are better done freezing to tie up chlorophyll with the water solubles. Evaporate all the way, scrape on to parchment paper and weigh it. You now have everything from the lupulin glands, all the alpha, beta, essential oils and aromatic hard and soft resins.
Experiment! Find what works effieciently for you! I've been having fun making this process very efficient and I will be selling my extracts to brewers in my area.

 

[moorehops]

Yeah, post-primary beer I meant, not wort.

So solubility of these solids is sufficient that you can use in the bottle without someone eating a hop nugget? Because I am thinking of these applications for postboil, myself.

Liquids are also easier for a user to measure, of course. I get what you're saying about the oils separating when you add it to beer from the ethanol extract, but then getting the extract into a roughly beer-like concentration of alcohol for delivery seems like a good alternative, even if you have to add 250ml to your beer or more... I dunno the delivery of a solid extract is hard for me to wrap my head around.

Oil/ethanol floats to the top doesnt mix well.
Resin extract sinks, then as it dissolves away oil it decants and mixes into the brew. Much like hops or pellets act in the brew but without the adsorption or the mush.

 

[OhSoHumuLonely]

If you are getting all the alpha acids, how are you getting isomerization when you add to cold/rt beer?

 

[OhSoHumuLonely]

Ohhh, nevermind. That is just for dry hopping, where dissolving alpha acids isn't necessary, right?

 

[fearwig]

Some people were talking about that earlier but I don't think you want isomerization here, that's just for bittering, and who has a problem getting enough bittering? I think all the nonsense about utilization is something for commercial BMC type brewers who want to squeeze an extra barrel's beer out of their hops. The advantage of this, to me, is A) take away the pain in the butt of dry hopping and the volume loss, B) get some more punch from your dry hops, which people have to use in much higher volumes than for bittering to have the effect they want. If you can get 4oz worth of dry hop flavor out of an extract made from 1oz of hops and it takes ten minutes instead of a week, that's a much bigger deal than the bittering side.

Ohhh, nevermind. That is just for dry hopping, right?

Oops yeah, guess you got it.

 

[moorehops]

No, if you want bittering you add the extract at the beginning of the boil. Do you not realize how much liquid volume is lost to hops. Plus the added taste of the plant matter and chlorophyll. Believe me, you would much rather your beer get its bitterness from the lupulin then from the other water solubles.
Once again you are simply removing the contaminants from the recipe. If you want different flavors, extract from different strains of hops.