Having serious oxidation issues bottling, please help

[olotti]

Sorry this may be a long post but I want to detail my procedure so it's known and maybe there's something I'm missing here.

So I've noticed this mostly with my hop heavy IPAs and dipas lately more than anything, I bottled an apa over a month ago that's still holding and a blonde 3 weeks ago that's the clearest beer I've ever made yet my hop heavy beers literally by day 10-14 are showing signs of oxidation mostly in a darker color change, lack of hop profile and increased back end bitterness almost harshness like there's literally no hop flavor anymore. I use Ro water and build it up in incase your wondering. So here's My bottling process so please let me know if you see any issues of why this is happening

So pitch beer and put in basement, then by day 5-7 I move the carboy upstairs to finish out and while of course the liquid moves there's no sloshing up the side of the carboy or bubbles forming so nothing that worries me that moving it is causing oxidation at this point. I'll dry hop by day 7, then again by day 10. Then pick up the carboy and move it to my outside fridge to cold crash, again no sloshing or obvious bubbling from oxygen, I keep the 3 piece Airlock on while cold crashing, this may be part of the problem as I've notice in the first 24 hrs of cold crashing the liquid is sucked down all the way to the bottom of the inner bell, there's still liquid above the bottom of the bell but just barely so I'll refill the airlock with stars an. Cold crash 48 hrs and bring the carboy inside and set it on the counter. Transfer to bottling bucket with a 6' siphon hose so it curls in the bottom of the bucket and again no obvious bubbling that would worry me and no bubbles in the siphon line itself. When done filling the bucket pick it up to the counter and cover the top with sanitized foil, attach my bottling wand to the spigot then start filling. I fill a bottle then put on an O2 barrier cap then set aside, I'll do this for 6 beers then crimp them all down and that's basically my whole process. I'll let the beers condition in my closet at 72 deg for 7-10 days then into the fridge they go and I've been getting noticeabl changes in the beer even while in the fridge say by day 14, I'm drinking some now that are 14 days since bottling been in the fridge 5-6 days and Im seeing changes just like the last two beers that to me are obvious oxidation issues. So I have no idea what's going on and why it's hitting these beers so fast, just coincidence they're hoppy beers and that's fueling it, idk. Anything you see in my process where I could be missing something. I'm so frustrated and disappointed because all the beers had a lot of potential, guess it's time to start kegging. Thanks for reading the long post I appreciate any help.

 

[kh54s10]

I can't say to the oxidation but are they carbonated? It sounds like you bottle conditioned for about 11 days then put them in the refrigerator. Mine are only sometimes carbonated at 2 weeks at 3 weeks they are good and taste better.

The only other place I can see anything happening is when you are dry hopping???

 

[olotti]

I can't say to the oxidation but are they carbonated? It sounds like you bottle conditioned for about 11 days then put them in the refrigerator. Mine are only sometimes carbonated at 2 weeks at 3 weeks they are good and taste better.

The only other place I can see anything happening is when you are dry hopping???

They are def carbonated, i mark the last 6 bottles I fill as tester bottles and I'll try those at day 7, 10 or 14 usually by day 10 they're clearly carbd, nice head and bubbles streaming up from the bottom of the glass. I'll let them sit in the fridge for 2-4 days then try one just to make sure before I put the rest in.

I've been trying the trend of dry hopping at the end of primary fermentation so day 5 usually using Conan or 1318 I'm on 4 th gen of both at this point, then dry hop again on day 7 or 8 let that sit at room temp for 2-3 days then move the carboy to the fridge to cold crash. By the time I bottle the first hop addition will have been in the beer for no more than 7 days. Could it be the opening of the bung and adding of two 3oz hop additions causing this, I add the hops through a funnel because usually they're all added together and they splash a little but I've read that couldn't really add enough oxygen to ruin a beer but it's made me think of just going back to one giant dry hop to see what the difference would be. Thanks for the reply.

 

[kh54s10]

I don't know how much this splashing does. I bag my dry hops, one ounce in a one gallon paint strainer bag. I get only one splash!

What is the taste? I always hear the description of wet cardboard. Usually no discussion of color. I wonder if it is something else.

 

[olotti]

I don't know how much this splashing does. I bag my dry hops, one ounce in a one gallon paint strainer bag. I get only one splash!

What is the taste? I always hear the description of wet cardboard. Usually no discussion of color. I wonder if it is something else.

The taste is just muted the nose may be fine but the taste especially on the back end doesn't carry through with the juicy hop flavor it's actually more sharp and bitter. From what I've read and experienced usually color changes first a noticeably darker beer than expected and then the hop flavor Is missing on the palate, which is usually next to go. The cardboard/sherry comes in later.

Weird thing thats confusing the heck out of me is that both the pale ale and blonde obviously less hoppy beers came out great and stayed that way using the same bottling technique I described above. So I brewed two dipas both effected by oxidation, then the blonde and pale ale and no such trace, then two IPAs the first like I mentioned has the same signs as the previous dipas while the other is still carbing but the samples at day 7 of conditioning are great. So I'm at a loss.

 

[flars]

Were the hops used in the IPAs fresh hops in sealed packages. Old hops can build off flavors similar to your description.

 

[kh54s10]

Since it is only your IPAs I am guessing that it is not an oxidation issue. But I have no idea what it would be. Bad hops? Too much hops?

 

[JordanKnudson]

I had bad oxidation issues when I was bottling as well, and generally only with hoppy beers. Some hop compounds oxidize very easily from what I understand, and the more hops you have, the more prone your beer is to that. I don't know exactly where in the process that happened to me, but I imagine it has to do with more frequent exposure to air (opening the fermentor multiple times to add dry hops), and then the small amount of oxygen introduced during bottling. As I said, not 100% sure exactly where the problem happens (or if it is even just a single part of the process that causes it), but since I started kegging, dry hopping in the keg, and doing CO2 purged closed-system transfers, I've not had any problems with this.

To kh54s10's comment, yes, oxidation causes noticeable color changes as well. The beer begins to darken, just like and apple or an avocado that is sliced and left exposed to air. It happens just as quickly as the off-flavors present themselves.

 

[olotti]

Were the hops used in the IPAs fresh hops in sealed packages. Old hops can build off flavors similar to your description.

I usually get my hops from farmhouse and they come vacuum sealed so I'm assuming they are fresh, they always smell really good.

 

[olotti]

I had bad oxidation issues when I was bottling as well, and generally only with hoppy beers. Some hop compounds oxidize very easily from what I understand, and the more hops you have, the more prone your beer is to that. I don't know exactly where in the process that happened to me, but I imagine it has to do with more frequent exposure to air (opening the fermentor multiple times to add dry hops), and then the small amount of oxygen introduced during bottling. As I said, not 100% sure exactly where the problem happens (or if it is even just a single part of the process that causes it), but since I started kegging, dry hopping in the keg, and doing CO2 purged closed-system transfers, I've not had any problems with this.

To kh54s10's comment, yes, oxidation causes noticeable color changes as well. The beer begins to darken, just like and apple or an avocado that is sliced and left exposed to air. It happens just as quickly as the off-flavors present themselves.

See this is what makes me think that no matter how careful I am as long as I bottle the beer will be exposed to O2 and I'm seriously careful about not doing anything that would further expose or introduce oxygen, I spend to much time and money on a batch to run the risk. I think until I get my keezer going I'm gonna back off on the hops a little and go back to doing one dry hop instead of two additions and just see if this doesn't at least help.

 

[m00ps]

I had this happen in a few hoppier beers ive made before. Got notably darker. Even comparing bottle to bottle looking through a light.

I was undecided on my last few brett IPAs ive done on whether I wanted to keg them or not since the brett yeast at the bottom really helps them change in the long run rather than degrade. I ended up purging the headspace in the bottling bucket and each individual bottle before filling. If you are still waiting on your kegging system, but can get the CO2 part of it, id jump on that as it could help you now too

 

[Pariah3j]

You could get you a bottle of C02 and and purge the top of fermentor of oxygen after every time you open it to hop, etc. ?

 

[KeninMN]

I strongly believe that you really have to try hard to oxidize a bottle-conditioned beer. I've actually run experiments at bottling time where I purposely added as much air as possible to the very last bottle and then set it aside for up to a year, alongside another bottle that had no discernable aeration. Side-by-side comparisons indicated no detectable difference between the two beers. Here is more from the head of QC at Dogfish Head:

Although bottle-conditioning typically doesn't change alcohol content all that much, it can help a beer age gracefully. The live yeast suppresses oxidation and the breakdown of flavors, potentially adding years to shelf life.

http://www.dogfish.com/community/blogfish/members/justin-williams/theyre-alive-bottle-conditioned-beers-get-a-complex-kiss-of-carbonation.htm

I suspect you have other process issues.

 

[JordanKnudson]

I strongly believe that you really have to try hard to oxidize a bottle-conditioned beer. I've actually run experiments at bottling time where I purposely added as much air as possible to the very last bottle and then set it aside for up to a year, alongside another bottle that had no discernable aeration. Side-by-side comparisons indicated no detectable difference between the two beers. Here is more from the head of QC at Dogfish Head:



http://www.dogfish.com/community/blogfish/members/justin-williams/theyre-alive-bottle-conditioned-beers-get-a-complex-kiss-of-carbonation.htm

I suspect you have other process issues.

I recently heard an interview (wish I could remember who, but someone of note) in which it was stated that the yeast only use roughly 75% of the oxygen in the head space of the bottle, which obviously leaves a bit left over to get into the beer.

I imagine you did your side-by-side experiment with something other than an IPA, since IPAs (American, at least) have so short a shelf life that comparing them after a year would be pointless. However, the OP is having this experience with hop-heavy beers exclusively, and it is most likely those easily oxidized hop compounds that are creating the problem. It may not be happening specifically at bottling, but there is a clear culprit. It could be oxygen exposure when opening the fermentor to dry hop, when transferring the beer, or during bottling, or (more likely) a little bit at each stage.

 

[jddevinn]

Then pick up the carboy and move it to my outside fridge to cold crash, again no sloshing or obvious bubbling from oxygen, I keep the 3 piece Airlock on while cold crashing, this may be part of the problem as I've notice in the first 24 hrs of cold crashing the liquid is sucked down all the way to the bottom of the inner bell, there's still liquid above the bottom of the bell but just barely so I'll refill the airlock with stars an.

As you cool the air and the beer inside the carboy the air volume shrinks creating a vacuum inside the carboy. Once the sanitizer in the airlock gets pulled into the fermenter air will start to be pulled in.

You should either not cold crash or cold crash under positive CO2 pressure.

Bottling does give a bit of leeway on oxygen uptake over kegging but only a little.

 

[olotti]

As you cool the air and the beer inside the carboy the air volume shrinks creating a vacuum inside the carboy. Once the sanitizer in the airlock gets pulled into the fermenter air will start to be pulled in.

You should either not cold crash or cold crash under positive CO2 pressure.

Bottling does give a bit of leeway on oxygen uptake over kegging but only a little.

I've heard using an S type airlock when cold crashing can prevent this suck back due to the design of the airlock. Not sure if this is true or not.

 

[unionrdr]

"S" type airlocks can give less fluid suck-back. But primary only lasting 7 days, I have to wonder, are you doing hydrometer tests to make sure it's don fermenting in the Double IPA's before dry hopping? The yeast finishing up fermentation could scrub hop aroma & flavor. The dry hop oils cling to the yeast & trub as it settles, loosing them in the trub/yeast at the bottom.
And I always dunk the caps, especially O2 barrier ones in Starsan before placing them on the bottles. Crimp, then tip the bottle to make sure the O2 barrier caps are wetted, as this is what activates them.
The one week primary could explain why the regular APA's & IPA's turn out better. Imperials & other high-gravity beers need more primary time to finish fermenting. And my bottled beers are better conditioned & have better carbonation at three weeks on average. With 1 week fridge time minimum, depending on the style.
And I've had beers oxidize before, but the color/clarity never suffered. But a beer will look darker as yeast & trub settle out, giving less reflectivity to light. They don't seem to darken as easily as fruit or veggies that are raw.

 

[jddevinn]

I've heard using an S type airlock when cold crashing can prevent this suck back due to the design of the airlock. Not sure if this is true or not.

Nope. The change in volume of air means something has to get sucked in, whether it is through the airlock or around it. If it is fully sealed then there would be a vacuum in the fermenter.

 

[KeninMN]

I imagine you did your side-by-side experiment with something other than an IPA, since IPAs (American, at least) have so short a shelf life that comparing them after a year would be pointless. However, the OP is having this experience with hop-heavy beers exclusively, and it is most likely those easily oxidized hop compounds that are creating the problem. It may not be happening specifically at bottling, but there is a clear culprit. It could be oxygen exposure when opening the fermentor to dry hop, when transferring the beer, or during bottling, or (more likely) a little bit at each stage.

I've done this experiment with IPAs. In fact, I have two year-old IPAs that are still fantastic. They are obviously different from when they were fresh, but still taste wonderful.

 

[olotti]

"S" type airlocks can give less fluid suck-back. But primary only lasting 7 days, I have to wonder, are you doing hydrometer tests to make sure it's don fermenting in the Double IPA's before dry hopping? The yeast finishing up fermentation could scrub hop aroma & flavor. The dry hop oils cling to the yeast & trub as it settles, loosing them in the trub/yeast at the bottom.
And I always dunk the caps, especially O2 barrier ones in Starsan before placing them on the bottles. Crimp, then tip the bottle to make sure the O2 barrier caps are wetted, as this is what activates them.
The one week primary could explain why the regular APA's & IPA's turn out better. Imperials & other high-gravity beers need more primary time to finish fermenting. And my bottled beers are better conditioned & have better carbonation at three weeks on average. With 1 week fridge time minimum, depending on the style.
And I've had beers oxidize before, but the color/clarity never suffered. But a beer will look darker as yeast & trub settle out, giving less reflectivity to light. They don't seem to darken as easily as fruit or veggies that are raw.

My primary time is usually 10 days. In trying to capture this NE style of IPA's the word is they usually do the first dry hop as primary fermentation dies down for me that's about day 5, then ill dry hop again around day 10, let that sit for 2 days and cold crash for 24 hrs then bottle. I'm always at FG by day 10 atleast that's what I've been experiencing and that's using a hydrometer to measure FG.

When bottling my caps sit in a dish of starsan, never tried the tipping technique though.

 

[olotti]

I strongly believe that you really have to try hard to oxidize a bottle-conditioned beer. I've actually run experiments at bottling time where I purposely added as much air as possible to the very last bottle and then set it aside for up to a year, alongside another bottle that had no discernable aeration. Side-by-side comparisons indicated no detectable difference between the two beers. Here is more from the head of QC at Dogfish Head:



http://www.dogfish.com/community/blogfish/members/justin-williams/theyre-alive-bottle-conditioned-beers-get-a-complex-kiss-of-carbonation.htm

I suspect you have other process issues.

So if this is the case and there is something else going on where do you think it would start. I'm just confused because if this was happening to every beer I've made lately ok I get it but its strictly been the last 3 IPA's where I went heavy handed, over 1lb of hops in each beer, that this issue has taken place and in the meantime the blonde and APA I made have been great showing none of this signs of the other beers. Brewing process and bottling process included just 24 hr cold crashes were the same for all the beers. But I'm all ears if you have other suggestions on where something may be going awry.

 

[KeninMN]

What is your water source?

 

[olotti]

What is your water source?

I use RO and build up the profile using bru'n water.

 

[KeninMN]

Are you directly measuring pH with a quality meter or just relying on the spreadsheet?

 

[olotti]

Are you directly measuring pH with a quality meter or just relying on the spreadsheet?

I do not have a pH meter at the moment so I'm just trusting in the program and the iut that I give it to spit out the correct pH. I use lactic acid to get my pH down to 5.2-5.4 range. Just curious but how would I not hit the correct predicted pH ifI add all the minerals and acid as the program suggests, what would throw it off from what the progrM predicts.

 

[KeninMN]

Because YMMV. The spreadsheets are a good tool to get you in range, but any number of things can happen to make the number they output different from what you actually have. If you're not measuring you're only guessing.

For what it's worth, I've never had any of the spreadsheets correctly predict my mash pH. I use a good quality meter and perform a 2-point calibration before every use. In every brew I've done since I started all grain brewing the spreadsheets have alway been 0.2 - 0.4 points off to the high side, so I would have been adding acid when I didn't need to.

 

[rhys333]

Sorry this may be a long post but I want to detail my procedure so it's known and maybe there's something I'm missing here.

So I've noticed this mostly with my hop heavy IPAs and dipas lately more than anything, I bottled an apa over a month ago that's still holding and a blonde 3 weeks ago that's the clearest beer I've ever made yet my hop heavy beers literally by day 10-14 are showing signs of oxidation mostly in a darker color change, lack of hop profile and increased back end bitterness almost harshness like there's literally no hop flavor anymore. I use Ro water and build it up in incase your wondering. So here's My bottling process so please let me know if you see any issues of why this is happening

So pitch beer and put in basement, then by day 5-7 I move the carboy upstairs to finish out and while of course the liquid moves there's no sloshing up the side of the carboy or bubbles forming so nothing that worries me that moving it is causing oxidation at this point. I'll dry hop by day 7, then again by day 10. Then pick up the carboy and move it to my outside fridge to cold crash, again no sloshing or obvious bubbling from oxygen, I keep the 3 piece Airlock on while cold crashing, this may be part of the problem as I've notice in the first 24 hrs of cold crashing the liquid is sucked down all the way to the bottom of the inner bell, there's still liquid above the bottom of the bell but just barely so I'll refill the airlock with stars an. Cold crash 48 hrs and bring the carboy inside and set it on the counter. Transfer to bottling bucket with a 6' siphon hose so it curls in the bottom of the bucket and again no obvious bubbling that would worry me and no bubbles in the siphon line itself. When done filling the bucket pick it up to the counter and cover the top with sanitized foil, attach my bottling wand to the spigot then start filling. I fill a bottle then put on an O2 barrier cap then set aside, I'll do this for 6 beers then crimp them all down and that's basically my whole process. I'll let the beers condition in my closet at 72 deg for 7-10 days then into the fridge they go and I've been getting noticeabl changes in the beer even while in the fridge say by day 14, I'm drinking some now that are 14 days since bottling been in the fridge 5-6 days and Im seeing changes just like the last two beers that to me are obvious oxidation issues. So I have no idea what's going on and why it's hitting these beers so fast, just coincidence they're hoppy beers and that's fueling it, idk. Anything you see in my process where I could be missing something. I'm so frustrated and disappointed because all the beers had a lot of potential, guess it's time to start kegging. Thanks for reading the long post I appreciate any help.

From your descriptions, I'm not getting oxidation so much as infection. If you're getting nice beers that seem to turn quickly, with hop characteristics disappearing and harsh bitterness forming over time, my first thought is an infection in your system somewhere. Replace your transfer tubing if you haven't yet. Disassemble to bottling bucket too, and let that spigot soak in a PBW or oxyclean.

On the other hand, if you're beers lack hop character and brightness from the get-go, and there's an harsh astringent quality right up front, then I would look at mash pH problems (assuming you do all-grain). Too high a pH results in tannin extraction from the grain (i.e.: astringency), and beers that seem flat or lacking in brightness. The Brewing Water Chemistry Primer in the Brew Science forum is a great resource for fixing this problem.

 

[olotti]

Because YMMV. The spreadsheets are a good tool to get you in range, but any number of things can happen to make the number they output different from what you actually have. If you're not measuring you're only guessing.

For what it's worth, I've never had any of the spreadsheets correctly predict my mash pH. I use a good quality meter and perform a 2-point calibration before every use. In every brew I've done since I started all grain brewing the spreadsheets have alway been 0.2 - 0.4 points off to the high side, so I would have been adding acid when I didn't need to.

Ok makes since. I just ordered the MW-102 meter, I was gonna brew Saturday but I'll prob wait now until I get the meter. I'm curious to see what the actual pH of the mash is or if it's even been close.

 

[KeninMN]

Here is more information on pH that you might find useful:

http://www.mbaa.com/districts/Northwest/Documents/BAMFORTH,%20pH%20in%20brewing.pdf

http://braukaiser.com/wiki/index.php/How_pH_affects_brewing#Inhibition_of_beer_spoilage_organisms

 

[eric19312]

The darkening beer thing...

Is it possible this is haze particles falling out of suspension in the bottle? As beer clears it tends to appear darker. Think about the progression in the carboy light when it is full of trub, dark when the trub falls, light again when yeast is going crazy, dark again when the yeast flocs out.

The flavors you are looking for may be hop oils adhered to yeast or other stuff in suspension. If they are the flavor you are seeking of course you will not like the beer as much once they settle to the bottom. When they drop you will be left with the bitter beer. You may not have noticed the bitterness before because the hop flavors can also be sweet. If the sweet hop flavors fell out the beer would seem more bitter.

Your solution would be as some of the NE style IPAs are recommending to re-suspend the hop oil globs. This is an issue with bottle conditioned beer however as you will be re-suspending too much yeast. I'd suggest force carbing the beer and then filling while still somewhat cloudy into bottles. These bottles could then be resuspended the way brewers are recommending treating their cans. Force carb, cap on foam, using an oxygen absorbing cap.

 

[rhys333]

I hadn't ready through the entire thread before my previous post, but I see now that others raise the pH issue.

olotti, I wouldn't be worried about brewing without a pH meter. I like to use EZ Water, and find that if I add all my salts to the main mash and shoot for 5.4 room temp pH estimate, I never have any issues. That said, I find predictions are more accurate if I exclude large amounts of roast and/or crystal malts from the mash and steep them separately. I'm also careful not to over-sparge and shoot for 75-80% efficiency max.

 

[olotti]

I hadn't ready through the entire thread before my previous post, but I see now that others raise the pH issue.

olotti, I wouldn't be worried about brewing without a pH meter. I like to use EZ Water, and find that if I add all my salts to the main mash and shoot for 5.4 room temp pH estimate, I never have any issues. That said, I find predictions are more accurate if I exclude large amounts of roast and/or crystal malts from the mash and steep them separately. I'm also careful not to over-sparge and shoot for 75-80% efficiency max.

I'm not saying it's not a pH issue but if that was the case wouldn't all the beers I make have an issue as all their pH values would be off and such is not the case I've made some good stuff all while using bru'n water. Other thing I'm getting now that the beer is 3 weeks old is the definite sherry character which is another key sign of oxidation, no phenols or anything that would make me think infection plus I just got all new bottling equipment, siphon, hose, spigot since the other stuff was getting old.

 

[daggers_nz]

I'm not saying it's not a pH issue but if that was the case wouldn't all the beers I make have an issue as all their pH values would be off a

you mentioned that your blonde was fine? The lower SRM (colour) accounts for a more alkaline mash pH so that would answer for any differences between that and say, an IPA with a slightly darker colour

 

[olotti]

you mentioned that your blonde was fine? The lower SRM (colour) accounts for a less alkaline mash pH so that would answer for any differences between that and say, an IPA with a slightly darker colour

Could u elaborate on this a little as like u say I have a blonde that's a month old and it's still killer and a pale ale only a couple left of those showing no signs of oxidation. I just started drinking my latest heavy dipa the last few days and it's two weeks old and it drinking real well now hence my confusion as this is a rebrew of one of the earlier beers that was oxidized but I changed my bottling technique for this beer. The last iipa I made it was picking up air of hops and trub during transfer to bottling bucket so I had to stop and restart it which Prob killed it whereas this ipa went like usual and real smooth