Bottling with the Help of Dry Ice

[PlinyTheMiddleAged]

All,

I've posted in a few different threads about what I do to minimize the exposure of my beers to oxygen. The background is that I had what I thought was pretty decent beer based on tasting what was in the bottling bucket; however, three weeks later, I'd have pretty nasty beer in my glass. Although I was shooting for IPAs, I was getting off colored (dark) crummy tasting beers. After discussing my problem with a local pro-brewer and tasting beers with him of various ages, I began my effort to minimize O2 exposure to see if this was my problem. However, I had no CO2 equipment and I did not want to spend a bunch of money if this was not my problem. So, I settled on using dry ice. Below is an outline of my bottling process.

Step 1: Sanitize bottles. I use my oven to bake my pre cleaned bottles. I cover the mouth of each bottle with aluminum foil and bake at 350ºF for about 1.5 hours. I then turn off the oven and leave the bottles to come back down to room temperature - usually overnight.

Step 2: Flush bottles, bottling bucket, hoses, wands, etc with CO2. I peel back the foil on the bottle, drop a good size piece of dry ice into each sterilized bottle, put the foil back in place, and let the dry ice sublimate. Honestly, I do not know how many volumes of CO2 I am flushing these bottles with - I think, based on my guesses of the dimensions of the pellet in the picture, that the chunk of dry ice weighed about 11 grams. This 11 grams will produce about 11 pints of CO2.

I also drop a couple of good handfuls of pellets in the bottling bucket - again, I don't measure how much I have used, but I'm pretty generous. I connect the sanitized hoses, wand, and valve to the bucket and let the CO2 flow through it all.

I let all of the above sit until the dry ice in the bottles and in the bucket has sublimated.

Step 3: Siphon the beer to the CO2 flushed bottling bucket. OK - here is where my process fails. I can't transfer without introducing oxygen into the fermenter. However, I know that when the beer gets to the bottling bucket, the CO2 protects the beer from further exposure. Sometimes I prime with carb drops; sometimes I use a priming solution.

Step 4: Fill the bottles with beer. Pretty simple. I am moving the beer from the CO2 flushed bottling bucket to a CO2 flushed bottle. Yes - when I am draining beer from the bottling bucket, I am letting air in; again, this process is not perfect.

Step 5: Drop a very small piece of dry ice into the now filled bottle. I do this to purge the head space in the bottle that is introduced when I remove the wand from the bottle. If the piece that you use is too big, you'll make a lot of CO2 bubbles that will overflow the bottle - so don't use too much. Place the cap on the bottle but do not crimp it down.

Step 6: After the dry ice has sublimated, crimp the top down.

Is this process perfect? Nope. Is it easier than buying a CO2 bottle, a keg, and all the associated fixtures and simply kegging? Probably not. However, if you think that you have problems with oxidation and you don't want to spend a bunch of money to see if that has a chance of solving your problem, give the dry ice a try. It has significantly improved my IPAs.

 

[ruger988]

Wow, I just santize my bottles with star-san and fill them with a bottling wand.... talk about some overkill. Whatever works for you though!!

 

[Yuri_Rage]

This appears to be an overly complex solution in search of a problem. As you may know, I have an affinity for complexity, but I'm going to criticize this particular method.

Oxygen exposure in a bottling bucket is a non-issue. The beer isn't there for long enough to oxidize. Careful racking will further prevent oxidation, which occurs most rapidly during transfers due to poorly sealed siphon lines and/or splashing. I simply recommend avoiding any racking, and bottling via siphon or adjustable spigot (a la Better Bottle spigot) on the primary fermenter.

Freshly fermented beer already has CO2 in it, which should help to create a CO2 rich environment in the headspace of a bottle (or carboy) as it comes out of solution during filling (there is really no such thing as purging without first pulling a vacuum).

If it makes you feel better, continue doing this, but I fail to see it as a best practice.

 

[PackerfaninSanDiego]

This is gotta be the most OVERKILL ever!!! You are taking the fun out of brewing/bottling beer! I bottled today.....all my bottles after each use, gets a good hot water soak and shake. I put them in my garage in a wooden crate, neck up. On bottling day I soak my bottles in Star-San as I am boiling my priming sugar mixture. I put the priming sugar in the freezer to get it cooled. As the priming sugar is cooling, I use my bottle washer on each bottle and then put it in the bottle tree. That's my process in a nutshell. KISS!

 

[dnslater]

Wow, I just santize my bottles with star-san and fill them with a bottling wand.... talk about some overkill. Whatever works for you though!!

My thought too.

 

[Hello]

Good lord, I'm lost. I thought star san did the trick.

 

[PlinyTheMiddleAged]

Is this overkill? Yes! I definitely agree that it is. But I had a real problem looking for a cheap solution. This is a suggestion for anyone who thinks they might have problem with oxidation but didn't want to buy a CO2 system without some proof that there would be a benefit.

I was being careful to minimize splashing during transfer to the bottling bucket but I was still getting what I thought was severely oxidized beer. A pro brewer in my area talked about keeping exposure of their IPAs to oxygen down to the parts per billion level. This was a way for me to minimize exposure to oxygen without investing in kegging equipment. And it worked.

If you think you have a problem with oxidation, give this a try. It solved my problem. Will I continue doing this? No - I'll switch over to kegging and then fill bottles from the keg as needed. If you don't have an oxidation problem, I'm not suggesting that you do this.

 

[flars]

if your only problem is oxidation, draining the beer into the bottles is most likely where it occurs. using a spring tipped bottling wand would take care of the problem, if you are not adding air at another point in the process.

 

[PlinyTheMiddleAged]

flars,

Thanks for the suggestion, but I do use a spring loaded valve on the tip of the bottling wand.

I'm not sure why my process led to such problems with oxidation. But if others suspect they're having similar problems, this is a fairly simple and cheap solution.

Thanks again!

 

[leesmith]

PlinyTheMiddleAged,

Great post! If I can find some dry ice, I'm gonna try this. From the blogs I've been reading I'm pretty sure anything you can do to limit the oxygen the better:

http://www.bear-flavored.com/2014/09/how-i-dry-hop-my-ipas-with-no-oxygen.html

http://www.themadfermentationist.com/2014/10/american-ipa-recipe-tips-and-tasting.html

Hop character (at least to me) fades real fast...malty beers don't seem to show signs of oxidation but by the time my bottled IPA's have been conditioned (I try to go no more than 10 days) the character has diminished enough for me to notice. The wow factor I get from the flat beer sample I take at bottling time is gone. They are not bad beers by any means, just not the beer I was hoping for.

In a response to a question about bottling IPA's on his recent IPA post Michael Tonsmeire says, "I brewed some solid IPAs and DIPAs before I kegged, but my worst batches now are better than my best batches then. During bottle conditioning the yeast scavenges some of the dissolved oxygen introduced during bottling, but the beer still spends a couple weeks warm exposed to the crown liner when it could be in the keg, cold, with extra dry hops. If you like the IPAs you are brewing, no reason to stop!"

 

[TheZymurgist]

You lost me at step 1. You bake your bottles?

 

[PlinyTheMiddleAged]

You lost me at step 1. You bake your bottles?

Yes I do bake my bottles. It's one of the bottle sanitizing options Palmer outlines in "How to Brew" - he has a table of temperature and duration needed. For me, it's a lot easier than StarSan and a bottling tree. Just cover the mouths with foil and put them in the oven for an hour. Turn off the oven and go to bed. Done.

 

[PlinyTheMiddleAged]

Hop character (at least to me) fades real fast...malty beers don't seem to show signs of oxidation but by the time my bottled IPA's have been conditioned (I try to go no more than 10 days) the character has diminished enough for me to notice. The wow factor I get from the flat beer sample I take at bottling time is gone. They are not bad beers by any means, just not the beer I was hoping for.

leesmith,

That's exactly the problem I was having with IPAs. Malty beers were fine (and I wouldn't go through this process for anything but an IPA). I'd have really tasty beers prior to bottling, but a few weeks later, I'd have nearly undrinkable, off colored beer in my bottles.

After attending a demonstration on the effects of oxidation at a local brewery (same IPA at different ages), I thought that it would be worth trying to minimize exposure to oxygen during the bottling process. However, I have no CO2 equipment or kegging equipment (and I don't really want to keg). So I thought I'd try dry ice.

And the process is not very complicated - drop a chunk of dry ice in a sanitized bottle and let it sit for a while, fill your bottle per usual, and drop in a small piece of dry ice to purge the headspace. Pretty easy, really. And more importantly, my IPAs went from barely drinkable to extremely good with a shelf life longer than I need (I drink them faster than they good bad).

Do I recommend this for all beers? Nope. But, if your IPAs suffer with off tastes and/or short shelf lives, this is a good way to see if oxidation is the source of your issues.

And thanks for those links! I'll read those over when I get a chance. Let me know if you try this and what your results are. Cheers!

 

[leesmith]

PlinyTheMiddleAged,

No problem for the links. These guys aren't saying bottled IPA's aren't as good because they have always kegged...they have done IPA's both ways and have come to some solid conclusions of their own on how to produce an aromatic, tasty IPA.

One consideration I've had lately was to buy a C02 tank in order to come up with a system to purge everything and then when I've got the money buy the equipment to keg.
With the tank you could transfer without any O2 exposure and devise a way to keep the bottling bucket under C02 also. Even if you didn't want to keg at all there may be a viable way to bottle without any O2 exposure. A DIY Blichmann type bottling gun or the real thing may be able to be worked into a system.

Just out of curiosity how much is the dried ice and how long does a bag/container last you?

 

[balrog]

Question: where do you buy dry ice that is considered clean enough to consume whatever is in/on the dry ice you are adding to the beer/bottles/buckets?

 

[PlinyTheMiddleAged]

One consideration I've had lately was to buy a C02 tank in order to come up with a system to purge everything and then when I've got the money buy the equipment to keg.
With the tank you could transfer without any O2 exposure and devise a way to keep the bottling bucket under C02 also. Even if you didn't want to keg at all there may be a viable way to bottle without any O2 exposure. A DIY Blichmann type bottling gun or the real thing may be able to be worked into a system.

That is probably my next step as well - follow a process similar to that used in kegging but without the keg. One could fill a bottling bucket with sanitizer and then force the sanitizer out with CO2 pressure and then add priming sugar. Do a pressure transfer from the fermenter to the CO2 flushed bottling bucket. Finally, using a Blichmann type gun, fill the bottles.

This is essentially what I am doing (more or less) with the dry ice just as a proof of concept. Since I have seen a HUGE improvement in my IPAs as a result, I am saving pennies to purchase equipment to accomplish the above.

Just out of curiosity how much is the dried ice and how long does a bag/container last you?

A bag of dry ice will last several hours. I buy about 5 pounds of pellets on bottling day (one dollar per pound) and apply it generously. I always have leftovers that end up in the trash. It won't last overnight.

 

[TheZymurgist]

leesmith,

That's exactly the problem I was having with IPAs. Malty beers were fine (and I wouldn't go through this process for anything but an IPA). I'd have really tasty beers prior to bottling, but a few weeks later, I'd have nearly undrinkable, off colored beer in my bottles.

This confuses me. If oxygenation is truly an issue for you, and not simply the degradation of hop aroma, then all of your beers would be changing color. Which would mean either you're introducing a ridiculous amount of oxygen during dry hopping, or you should be doing this with all of your batches. If you are introducing oxygen at dry hopping, I'm not sure how this process would fix that.

 

[testingapril]

I like the ingenuity here. O2 makes for lousy IPAs for sure.

Couple of process improvements you could make if you need to go even further.

1. Ferment in Better Bottles and get one of those CO2 injectors and rig up a valve on one of those orange caps and push the beer out with CO2. If you are using carb drops, you could bottle straight out of the fermenter this way and have no O2 exposure.

2. Use #1 and a bottling bucket, but drop some of the dry ice pellets in the bottling bucket as you bottle, that will keep a constant layer of co2 emanating from the beer which will be more protective than the proverbial, but mostly mythical "CO2 blanket." and the volume of CO2 produce will reduce oxygen ingress into the bottling bucket. Use a loose lid to keep the gas to gas interface space to a minimum. May need to watch out for lost co2 with this method, may have to up your carbonation a bit

3. Use oxygen absorbing caps. I've found they make a significant difference for aged beers, so I'm sure there's some benefit to using them short term as well. They aren't that much more expensive anyway.

 

[testingapril]

Question: where do you buy dry ice that is considered clean enough to consume whatever is in/on the dry ice you are adding to the beer/bottles/buckets?

It's available in grocery stores near me. I believe it's intended for use with ice cream and other food creations.

 

[PlinyTheMiddleAged]

TheZymurgist,

I brew two kinds of beers - stouts and IPAs. Perhaps I don't notice the color change on my stouts since they are already black. The IPAs are light enough that they definitely changed color between the bottling bucket and my glass.

And I think you're right, I must have been introducing ridiculous amounts of oxygen during bottling. Other folks in the oxidation demonstration that I attended had similar experiences with their IPAs (this demo was held at a West Coast IPA centric brewery). Maybe we all just had really poor bottling practices. But, from what I understand, IPAs are particularly sensitive to oxidation. My personal experience supports this.

Whether the cause was a really crummy process by me and the others attending the oxidation discussion or an extreme sensitivity of IPAs to oxidation, using dry ice as I've described solved the problem.

As an aside, I have always tried to minimize splashing during transfer to bottling bucket and when bottling. In spite of this, I never got an IPA that was really great after bottle conditioning. Now I do. Stouts were always fine.

 

[processhead]

It sounds like you have concluded that your beer tastes off due to oxidation during your bottling process.

Is that really the cause?

Find someone who can keg your next batch, and see if you can taste a marked improvement.

 

[PlinyTheMiddleAged]

It sounds like you have concluded that your beer tastes off due to oxidation during your bottling process.

Is that really the cause?

Find someone who can keg your next batch, and see if you see and taste a marked improvement.

Processhead,

You are correct, I have concluded that my problem was oxidation during bottling but I have not proved it conclusively.

I considered looking for a volunteer to keg a batch for me. I had someone lined up earlier this year, but he went away to college. He usually doesn't have much slack in his kegging schedule though (being a college kid, his kegs are usually in the process of being emptied and then immediately refilled).

 

[PlinyTheMiddleAged]

I like the ingenuity here. O2 makes for lousy IPAs for sure.

Couple of process improvements you could make if you need to go even further.

1. Ferment in Better Bottles and get one of those CO2 injectors and rig up a valve on one of those orange caps and push the beer out with CO2. If you are using carb drops, you could bottle straight out of the fermenter this way and have no O2 exposure.

2. Use #1 and a bottling bucket, but drop some of the dry ice pellets in the bottling bucket as you bottle, that will keep a constant layer of co2 emanating from the beer which will be more protective than the proverbial, but mostly mythical "CO2 blanket." and the volume of CO2 produce will reduce oxygen ingress into the bottling bucket. Use a loose lid to keep the gas to gas interface space to a minimum. May need to watch out for lost co2 with this method, may have to up your carbonation a bit

3. Use oxygen absorbing caps. I've found they make a significant difference for aged beers, so I'm sure there's some benefit to using them short term as well. They aren't that much more expensive anyway.

Testingapril,

1) Good idea. I really like bottling and have no room for a kegerator, so any way to keep O2 away from my IPAs is a good idea - skipping the transfer to the bottling bucket is a good idea.

2) Using dry ice to replenish the headspace in the bottling bucket during bottling is also a good idea. And I agree - the often repeated myth of the protective CO2 blanket is just that - a myth. Gases don't work that way. They diffuse no matter what. I'll post an interesting link later that clearly demonstrates this.

3) I usually use oxygen absorbing caps. I never noticed a benefit. My IPAs still suffered. I must really stink at bottling!!!

 

[T-Wayne]

This is an interesting read. Its got that going for it, but I do have to agree with others, it seems as though it may be overkill.

 

[PlinyTheMiddleAged]

Diffusion of gases of different densities - an interesting demonstration on YouTube.

http://youtu.be/_oLPBnhOCjM

This demo used bromine and air. Bromine is about 7 times more dense than air (if I recall correctly). CO2 is about 1.5 times more dense than air; therefore CO2 and air will mix faster than air and bromine.

From the demo, one can infer that once the CO2 contacts air, the O2 from the air will get to the beer which may result in oxidation. The ways to minimize exposure to oxygen are to keep the contact area between air and CO2 small - a carboy is better than a bucket. If you pull the stopper out of a carboy, you'll have a lot smaller contact area than you'd have if you pulled the lid off of a bucket. The second is time - keeping the airlock out of a carboy for one minute will lead to a lot less O2 being introduced than if you leave it out for 30 minutes. There are also effects from temperature and gas density as well. The example shows diffusion between gases across the entire top surface of the container (like a bucket). The diffusion would take a lot longer if the gases had to pass through a narrow neck (like a carboy).

Will you always get oxidation from exposing your CO2 blanketed beer to air? Nope. But my experience tells me that my IPAs are very sensitive to the introduction of O2. Like I said earlier, maybe my bottling process is really bad. Regardless, using dry ice as a crutch seems to have addressed the problem (although as processhead has pointed out, a friendly local brewer with a keg to spare would help finalize my conclusion concerning oxidation).

 

[TheZymurgist]

Diffusion of gases of different densities - an interesting demonstration on YouTube.

http://youtu.be/_oLPBnhOCjM

This demo used bromine and air. Bromine is about 7 times more dense than air (if I recall correctly). CO2 is about 1.5 times more dense than air; therefore CO2 and air will mix faster than air and bromine.

From the demo, one can infer that once the CO2 contacts air, the O2 from the air will get to the beer which may result in oxidation. The ways to minimize exposure to oxygen are to keep the contact area between air and CO2 small - a carboy is better than a bucket. If you pull the stopper out of a carboy, you'll have a lot smaller contact area than you'd have if you pulled the lid off of a bucket. The second is time - keeping the airlock out of a carboy for one minute will lead to a lot less O2 being introduced than if you leave it out for 30 minutes. There are also effects from temperature and gas density as well. The example shows diffusion between gases across the entire top surface of the container (like a bucket). The diffusion would take a lot longer if the gases had to pass through a narrow neck (like a carboy).

Will you always get oxidation from exposing your CO2 blanketed beer to air? Nope. But my experience tells me that my IPAs are very sensitive to the introduction of O2. Like I said earlier, maybe my bottling process is really bad. Regardless, using dry ice as a crutch seems to have addressed the problem (although as processhead has pointed out, a friendly local brewer with a keg to spare would help finalize my conclusion concerning oxidation).

That's really great video! I've had issues with the whole "CO2 Blanket" theory, and that just confirms it. When you add in the fact that the environment we're working in doesn't have perfectly still air, that creates a host of other issues.

As to IPAs being more sensitive to O2, that's true but only as it pertains to hop aroma. What you're describing, is oxydation, as evidenced by the change in color. IPAs are no more susceptible to oxydation than any other beer, which is why I stated that either you have an issue at *dry hopping* and not at bottling (which would not be fixed by this method) or that all of your beers are likely to experience oxydation. It's true that you're more likely to notice it in an IPA than a stout, given that the stout is dark to begin with, and that it's likely any flavors related to oxydation will be masked better by the stout.

My only point is that your issue seems to be fairly singular, as I think very few experience oxydation on the levels that you're describing, and that I'm sure there is an easier, less expensive way to fix the problem.

 

[PlinyTheMiddleAged]

This is an interesting read. Its got that going for it, but I do have to agree with others, it seems as though it may be overkill.

If you liked West Coast IPAs as much as I do but drank beers as bad as the ones that were coming out of my bottles, you'd also go to great lengths to address it!

Is it overkill? Most definitely! If I knew where to pull back a little and still have the same level of success of producing decent IPAs, I would do so. However, I'd rather not be faced with drinking another 5 gallons of sherry flavored brown IPA (shudder). Bottled CO2 and filling bottles from a keg are in my near future. The process of using dry ice during bottling was the proof of concept that I needed to nudge me in that direction.

Cheers!

 

[rafaelpinto]

I tried this method on a dry hopped saison I brewed a couple months ago. The hop aroma was there, but behind the saison aroma. In the end, the saison came more hoppy than my IPAs.

I will brew an IPA this week and intend to use dry ice again. I experience all the problems you list with my hoppy beers. Must be O2.

 

[Spartan1979]

It's available in grocery stores near me. I believe it's intended for use with ice cream and other food creations.

As you said, WITH ice cream, not in ice cream. I've read other sources that state dry ice is fairly dirty. It's not made to be consumed.

 

[PlinyTheMiddleAged]

Any product (including dry ice) that is used with food must be food grade.

 

[TheZymurgist]

Any product (including dry ice) that is used with food must be food grade.

I think it's any product that's used in food must be food grade, but I'm curious what your source is.

 

[hunter_le five]

Dry ice generally doesn't come in direct physical contact with food, when used for food purposes.

 

[steveoatley]

" Food Grade "

Also allows for a certain amount of 'bug' parts per million.

I did use Dry Ice a while back to mix a Cider with a Mead.

I did find in my research that Food Grade means what you might think and
There is Medical Grade Dry Ice - I could not find a supplier for it anywhere

I took five pounds of Dry Ice, pounded it into small chucks, dropped most of
chucks into a Carboy, then gently poured my mead & cider into the carboy to
make a Cyser.
I figured I have made at least 5 gallons of CO2 - more than enough to purge a
Carboy of O2

I did notice small "darker" partials in the CO2 chunk ( visible )- they just seemed darker, not like dirt, no partials/dirt or chucks of "stuff" were found later, when I racked into a keg.

https://www.homebrewtalk.com/f13/dry-ice-prevent-oxidization-during-racking-225825/


just my 2 cents

 

[PlinyTheMiddleAged]

I think it's any product that's used in food must be food grade, but I'm curious what your source is.

TheZymurgist,

If you check the FDA website, there's a flowchart that describes the decision process for approving food additives - the first decision point is something like: "is it reasonable that the product will become a component of food given its intended use". I'd say that since lots of folks use dry ice to cool food, it would be reasonable that as the dry ice sublimates, any contaminants could be deposited in or on the food. Plus, since it is not uncommon for people to put dry ice in punch bowls (for a "witch's brew" kind of thing) it is reasonable that dry ice (and anything in the dry ice) will become a component of food.

That's the way I read it, at least.

Cheers!

 

[PlinyTheMiddleAged]

I tried this method on a dry hopped saison I brewed a couple months ago. The hop aroma was there, but behind the saison aroma. In the end, the saison came more hoppy than my IPAs.

I will brew an IPA this week and intend to use dry ice again. I experience all the problems you list with my hoppy beers. Must be O2.

rafaelpinto,

Let us know how it works out for you! I bottled a great tasting Pliny the Elder clone yesterday using this method. Hopefully, when I pour it in two or three weeks, it'll still taste great. I know that the last time I brewed and bottled this, the beer was bad within days of being carbonated. That great, bitter, enamel etching hoppiness that Pliny the Elder is known for was not there.

I'm guessing that by using dry ice to flush the bottling equipment, and by using oxygen absorbing caps, this batch will have will a LOT better flavor, aroma, and shelf life.

And, I'm looking for a CO2 bottle and kegging equipment too. Probably going to ask Santa to see if he can swing it.

I'll let you know how mine turns out in a few weeks.

Cheers!

 

[PlinyTheMiddleAged]

Double post

 

[testingapril]

As you said, WITH ice cream, not in ice cream. I've read other sources that state dry ice is fairly dirty. It's not made to be consumed.

Penguin Brand Dry Ice would disagree. This is the brand that is sold in most grocery stores and their website actually provides recipes and the like for using it in cocktails and punch.

http://www.dryiceideas.com/more-safety-tips-for-using-dry-ice-in-beverages/

Also, FAQ says it's not toxic:

http://www.dryiceideas.com/faq/

Food grade doesn't mean sanitary, but -79C and pure CO2 environment is extremely unlikely to harbor beer infectors.

 

[fantomlord]

2 comments:

1. I deal with dry ice all the time at work...I would not put it into my beer. (a halloween punch, maybe, but as a novelty)
2. The word you guys are all looking for is "sublimes" {steps off soap box}

 

[rafaelpinto]

1. I deal with dry ice all the time at work...I would not put it into my beer. (a halloween punch, maybe, but as a novelty)

Is it unhealthy?

 

[kh54s10]

The main problem I have with all this overkill is that it might determine if oxidation is the problem, but does not determine how it is happening. So, you are stuck using co2 to bottle or you will have to go back and have oxidized beers.

When you say that other styles do not show the problem it says to me that oxidation is NOT your problem. At least not introduced during the bottling process.