Repeated Oxidation

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chieftain

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Greetings all,

I've been homebrewing for 6 months or so, since a buddy got me into it. Have really benefited from all the knowledge and tips shared on this site.

I mostly brew IPAs and DIPAs - started with extract-based versions and recently moved up to all-grain BIAB. Unfortunately my beers are consistently oxidizing after several weeks in the bottle, which is really frustrating. After reading the numerous threads on this subject, I'm still at a loss, and hoping someone may have an answer.

I've got 6-7 brews under my belt, usually in the 3-4.5 gallon range. My process is pretty standard. In general, after the boil I cool the wort and transfer to a bucket or carboy. Pitch the yeast at target temp and set it aside for 2 weeks or so at 68-70 degrees. I usually dry-hop for an additional week. I used a secondary for the first few brews, but stopped doing that out of concern it was contributing to the oxidation. Once fermented, I transfer the beer to a bottling bucket with an auto-siphon, careful to avoid any air in the line. I add the priming sugar dissolved in water, and bottle via a spring loaded bottle filler that is connected to the bottling spigot via hose. For the first 3-4 brews, I didn't put a cap immediately on each bottle after filling them, but waited until all of the bombers were full to cap them. I've since changed that approach, to no avail.

So I feel like I'm doing everything I can do, but my beers are still noticeably darkening after 3 weeks in the bottle, with the nice hoppy flavors being replaced by the dreaded sherry/cardboard taste. Kegging is not really an option, I'd like to make bottling work if at all possible. Any ideas?
 

rnm410

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I see a few things worth pointing out.

-Oxygen contact at liquid interface when transferring to bottling bucket.
-Dissolved oxygen in the water used for priming sugar, are you boiling to sanitize your sugar/water effectively deaerating it.
-Note yeast still active in the bottle will scavenge some oxygen.
-Use oxygen scavenging bottle caps.
-Blanket your bottling bucket under co2.
-Keep skipping the secondary.
 

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So you're generally doing three weeks in a fermenter, opening the bucket at day 14 or so, for dryhopping?

Have you considered dryhopping once fermentation ends, for 5 days or so, and then packaging the beer at that point? For me, that's often day 14 or sooner.
 
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chieftain

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I see a few things worth pointing out.

-Oxygen contact at liquid interface when transferring to bottling bucket.
-Dissolved oxygen in the water used for priming sugar, are you boiling to sanitize your sugar/water effectively deaerating it.
-Note yeast still active in the bottle will scavenge some oxygen.
-Use oxygen scavenging bottle caps.
-Blanket your bottling bucket under co2.
-Keep skipping the secondary.

Thanks for the response. I should have clarified that I do boil the priming sugar in the water and then cool it before adding. I started out adding this mixture to the bottling bucket after I transferred the beer from primary, but in the last two batches I added it first to minimize the stirring required to mix things thoroughly.

I have used oxygen scavenging caps for the last two brews. One of them was a porter, which hasn't shown any problems. The other was the El Jefe clone from Mitch Steele's book, and it has started to show oxidation problems.

I am considering picking up a Co2 tank and regulator to purge the bottling bucket and bottles, so good to know that you think it could help.
 
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chieftain

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So you're generally doing three weeks in a fermenter, opening the bucket at day 14 or so, for dryhopping?

Have you considered dryhopping once fermentation ends, for 5 days or so, and then packaging the beer at that point? For me, that's often day 14 or sooner.

yep, that's generally the case. I'm definitely not set on waiting 14 days to dry hop, I just thought that was a good amount of time to allow the yeast to do its thing and perform post-fermentation clean-up. I think I read one of your posts stating that this clean-up only takes a day or two post-fermentation? So you'd suggest dry-hopping around day 9?
 
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chieftain

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Also neglected to mention that I've drank multiple bombers from each brew session in the 2 weeks post-bottling (yes, I'm pretty impatient) and they've all tasted pretty good. One in particular, which was my own concoction of pale malt hopped with Mosaic/Citra/Amarillo, and fermented with Vermont Ale Yeast, was incredibly fruity and juicy...up until 3 weeks, after which it darkened up rapidly and became undrinkable.
 

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yep, that's generally the case. I'm definitely not set on waiting 14 days to dry hop, I just thought that was a good amount of time to allow the yeast to do its thing and perform post-fermentation clean-up. I think I read one of your posts stating that this clean-up only takes a day or two post-fermentation? So you'd suggest dry-hopping around day 9?

When fermentation is done, and the beer is clearing, it is a good time to dryhop. that could be day 5 or day 9- it depends on the yeast strain a lot of the time. For example, some yeast strains take forever to start to fall out, while others will fall out sooner. I'd go with "done fermenting +/- 3 days" as a general rule of thumb for IPAs and pale ales.
 
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chieftain

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When fermentation is done, and the beer is clearing, it is a good time to dryhop. that could be day 5 or day 9- it depends on the yeast strain a lot of the time. For example, some yeast strains take forever to start to fall out, while others will fall out sooner. I'd go with "done fermenting +/- 3 days" as a general rule of thumb for IPAs and pale ales.

Ok thanks for the suggestion. I'll try dry-hopping on a shorter time table than what I've been doing.
 

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During transfer and at bottling do you have an airtight connection with your auto siphon/bottling wand and hoses? No string of very tiny bubbles or sound coming from the connections?
 

rnm410

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Thanks for the response. I should have clarified that I do boil the priming sugar in the water and then cool it before adding. I started out adding this mixture to the bottling bucket after I transferred the beer from primary, but in the last two batches I added it first to minimize the stirring required to mix things thoroughly.

I have used oxygen scavenging caps for the last two brews. One of them was a porter, which hasn't shown any problems. The other was the El Jefe clone from Mitch Steele's book, and it has started to show oxidation problems.

I am considering picking up a Co2 tank and regulator to purge the bottling bucket and bottles, so good to know that you think it could help.

It would be nit picking at that point, I dont know if buying a tank would be necessary. Route your blow off tube from the primary into your bottling bucket?
 
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chieftain

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During transfer and at bottling do you have an airtight connection with your auto siphon/bottling wand and hoses? No string of very tiny bubbles or sound coming from the connections?

yes. I have an inch or so of Star San solution instead the bigger part of the auto siphon, which creates an airtight seal.
 
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chieftain

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It would be nit picking at that point, I dont know if buying a tank would be necessary. Route your blow off tube from the primary into your bottling bucket?

Yeah unfortunately that probably won't work cause I've got a couple rug-rats running amok all the time and limited space to store fermenters.
 
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chieftain

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So to provide some visual indication of how the oxidation is affecting my brews, here is a photo of an IPA (based on Pliny, but lower ABV) I bottled on 3/6. According to Beersmith, as brewed it came in around SRM 6.4. I didn't get a photo the day of bottling, unfortunately.

Based on past experience it's after the 2 week mark that the beer starts to oxidize, so I'll post another photo in a week. The primary difference in bottling this batch was to allow the beer to foam up over the top of the bottle before placing a cap on top.

20160318_201332.jpg
 
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chieftain

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And here is the same beer approximately 2 weeks later, on April 1st. Pic taken at same time of day, same lighting. Not sure if the color has changed much, certainly not nearly as dramatically as previous beers had. So maybe capping on the foam made the difference.

Taste-wise the beer isn't as good as I'd like, the hops are fairly muted and the overall flavor seems muddy, for lack of a better word.

20160401_182738.jpg
 
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chieftain

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In your last two post what are you calling oxidation?
Visual?
Taste?
...

Both. Previous IPAs/APAs I've brewed have darkened considerably - they would start at something like 4-6 SRM and end up at like 15 SRM. And the taste would worsen significantly. They became more caramel/sherry-like. The hops totally disappeared in the beer too.
 

rnm410

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-Post your beer recipe please.
-I overlooked yoopers post, she brings a good point up. Dry hop while some fermentation activity is still happening in the primary, yeasties are good at absorbing oxygen. When you add the hops and there is still some activity, say the conditioning phase, yeast will scavenge oxygen and remove some, if any oxidized off products.
-Post 13 and 14 are you calling that SRM darkening?
 
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chieftain

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-Post your beer recipe please.
-I overlooked yoopers post, she brings a good point up. Dry hop while some fermentation activity is still happening in the primary, yeasties are good at absorbing oxygen. When you add the hops and there is still some activity, say the conditioning phase, yeast will scavenge oxygen and remove some, if any oxidized off products.
-Post 13 and 14 are you calling that SRM darkening?

Answering your last question first, no, that is not the type of darkening I have seen previously.

Here's one for an APA I did back in January, that only used a hopstand for bittering and flavor. I believe I left it in the fermenter for 3 weeks total, with a secondary of 1 week (I've since stopped using a secondary). It was pretty good one week after bottling. Major darkening and off flavors after 3 weeks in the bottle. No pics unfortunately.

Grains to Steep
8.0 oz Caramel/Crystal Malt - 60L (60.0 SRM) Grain 1 5.9 %

Boil Ingredients
3 lbs Light Dry Extract (4.0 SRM) Dry Extract 2 35.3 %
5 lbs Pale Liquid Extract [Boil for 20 min](4.0 SRM) Extract 3 58.8 %

Steeped Hops
0.50 oz Cascade [5.50 %] - Steep/Whirlpool 30.0 min Hop 4 2.4 IBUs
0.50 oz Cascade [5.50 %] - Steep/Whirlpool 60.0 min Hop 5 3.2 IBUs
0.50 oz Centennial [10.00 %] - Steep/Whirlpool 60.0 min Hop 6 5.8 IBUs
0.50 oz Centennial [10.00 %] - Steep/Whirlpool 30.0 min Hop 7 4.4 IBUs
0.50 oz Citra [12.00 %] - Steep/Whirlpool 60.0 min Hop 8 6.9 IBUs
0.50 oz Citra [12.00 %] - Steep/Whirlpool 30.0 min Hop 9 5.3 IBUs
0.30 oz Amarillo [9.20 %] - Steep/Whirlpool 60.0 min Hop 10 3.2 IBUs
 
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chieftain

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-Post your beer recipe please.
-I overlooked yoopers post, she brings a good point up. Dry hop while some fermentation activity is still happening in the primary, yeasties are good at absorbing oxygen. When you add the hops and there is still some activity, say the conditioning phase, yeast will scavenge oxygen and remove some, if any oxidized off products.
-Post 13 and 14 are you calling that SRM darkening?

Here's another extract-based recipe that darkened considerably over the course of 3 weeks in the bottle:

Grains to Steep
8.0 oz Caramel/Crystal Malt - 40L (40.0 SRM) Grain 3 5.4 %

Boil Ingredients
1 lbs Light Dry Extract (3.0 SRM) Dry Extract 4 10.8 %
1 lbs 12.0 oz Corn Sugar (Dextrose) (0.0 SRM) Sugar 5 18.9 %
0.60 oz Amarillo [9.20 %] - Boil 60.0 min Hop 6 13.1 IBUs
0.60 oz Mosaic (HBC 369) [12.25 %] - Boil 60.0 min Hop 7 17.4 IBUs
0.50 oz Amarillo [9.20 %] - Boil 20.0 min Hop 8 6.6 IBUs
0.50 oz Citra [12.00 %] - Boil 20.0 min Hop 9 8.6 IBUs
0.50 oz Mosaic (HBC 369) [12.25 %] - Boil 20.0 min Hop 10 8.8 IBUs
6 lbs Pale Liquid Extract [Boil for 15 min](4.0 SRM) Extract 11 64.9 %

Steeped Hops
0.50 oz Amarillo [9.20 %] - Steep/Whirlpool 30.0 min Hop 12 4.2 IBUs
0.50 oz Citra [12.00 %] - Steep/Whirlpool 30.0 min Hop 13 5.5 IBUs
0.50 oz Mosaic (HBC 369) [12.25 %] - Steep/Whirlpool 30.0 min Hop 14 5.6 IBUs
◯ Estimated Post Boil Vol: 2.71 gal and Est Post Boil Gravity: 1.076 SG
 

rnm410

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I've never worked with extract, all extract beers I've tasted do have that oxidized twinge to them. Maybe we will let someone else chime in and help out.

One thing I have noticed in IPAs both commercial and homebrew is the effect of crystal malt and hop fade leading to muddled taste and oxidized flavors. Try carapils or a lighter crystal (10-20) in future batches if you haven't already.
 

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Do you use the same brand of extract each time or purchase from the same place each time? Have you looked into the freshness of the extract you are using ?
 
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chieftain

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I've never worked with extract, all extract beers I've tasted do have that oxidized twinge to them. Maybe we will let someone else chime in and help out.

One thing I have noticed in IPAs both commercial and homebrew is the effect of crystal malt and hop fade leading to muddled taste and oxidized flavors. Try carapils or a lighter crystal (10-20) in future batches if you haven't already.

That's an interesting idea. I've since switched to all-grain, and the Pliny was the first one I did, so perhaps this will make the difference. I just did a Double Sunshine clone that is very light and extremely hoppy, so this will be a good test case. It did have a bit of 60 crystal in it.

Also, I went back and looked at the first recipe I brewed - a Sculpin Clone without any crystal. I don't recall it darkening or showing the oxidized flavors ever.
 
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chieftain

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Do you use the same brand of extract each time or purchase from the same place each time? Have you looked into the freshness of the extract you are using ?

I believe they were mostly Briess extracts purchased from Northern Brewer or MoreBeer, so should have been fresh, right?
 

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When fermentation is done, and the beer is clearing, it is a good time to dryhop. that could be day 5 or day 9- it depends on the yeast strain a lot of the time. For example, some yeast strains take forever to start to fall out, while others will fall out sooner. I'd go with "done fermenting +/- 3 days" as a general rule of thumb for IPAs and pale ales.


Not to get too far off topic, but could that be applied to fruit beers as well? I've always done three weeks in the primary (no secondary, except for fruit) and I usually added the hops or fruit after the 14th day, then 3-7 days later, I'm kegging.


Is the darkening of an IPA a good indication of oxidation? My last IPA is a lot darker than usual. The color never changed from the keg, but the few I bottled from that keg has. The aroma is very faint and there's hardly any flavor there.
 

rnm410

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I do not know of darkening related oxidation, I will research into this. I do know of haze producing oxidation reactions though, those sometimes can come off as darkening to an extent.
 

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Not to get too far off topic, but could that be applied to fruit beers as well? I've always done three weeks in the primary (no secondary, except for fruit) and I usually added the hops or fruit after the 14th day, then 3-7 days later, I'm kegging.


Is the darkening of an IPA a good indication of oxidation? My last IPA is a lot darker than usual. The color never changed from the keg, but the few I bottled from that keg has. The aroma is very faint and there's hardly any flavor there.

Yes, I would assume fruit beers would be similar- except that adding fruit generally creates some fermentation and perhaps the oxidation risk would be minimized? I'm no expert on that, as I rarely make fruit beers, but I am a winemaker and adding fruit does usually kick off a secondary fermentation.

Darkening is usually one of the first signs of oxidation, actually. Long before flavor changes much, the beer will darken a bit and then start to stale a bit. A bit later on, it will take on "sherry" like flavors or brandy-like notes, or even a hint of metallic flavor in beers with darker roast malts, and when it's much worse is when you get the classic "cardboard" flavors that are most well known. The beer is very far gone by that point, so those "cardboard" flavors aren't as common.

Early oxidation is the most common flaw present in most of the beers I judge in competition, but many brewers who don't know the classic early signs don't know that. I think they are looking for "wet cardboard", and not early staling type of reactions and flavors.
 

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I bottled for the last 8-9 years until I worked into kegging last year. Never noticed any consistent problems...except for hop-centric beers. Had some beers that were fairly pale / delicate like saisons that even 6-8 months later may not have been quite 100% fresh, but still very tasty...but hoppy beers generally seemed to muddy up into the same kind of sticky-sweet hop flavor and darken some in color. One thing that was interesting to me was a handful of bottles from batches would be fine....but the majority of them were so afflicted.


The first beer I kegged was a white IPA. We were over on volume, so we bottled 1gal the same way we normally did (with an exposed bottling bucket, no purging of bottles or anything, etc) and kegged the rest. I didn't have the hardware yet to do a forced transfer into the keg, so I ran some CO2 into the keg with a hose, and gave it a few blasts as it was racking in via siphon as well. The kegged beer ended up great - crisp, bright hop flavor, to where you could pick out different characteristics of different hops. We just opened a bottled version at a recent brewday and did a side-by-side...I tasted the same old sticky-sweet + muted, muddied hop flavor in that one. It appeared a bit darker than the kegged version, though I don't think my buddy had the bottle crashing in the fridge for very long and it wasn't as clear. Pic: https://goo.gl/photos/keSHBnFqhJA4dTHPA


If you don't think you'll end up kegging, you can still get a CO2 tank as you had mused earlier, and one thing I would also throw out for consideration is to get one corny keg and use that as your bottling bucket. You would then have a few options here as to how far you'd want to go to minimize O2 exposure, but they're probably all better than your current process. On the more basic end would be to still dry-hop as you do now, put priming sugar solution in bottom of keg, attempt to do some amount of purging of headspace via CO2, and with the lid on the keg and the relief valve open, rack in through the beer out tube from your fermenter using CO2 to push the beer. Then you could use CO2 + a picnic tap + bottling wand or some similar setup to bottle.


It's an equipment hit (tank, keg, quick disconnects, etc), and CO2 isn't free, but if there's a chance you do want to advance to kegging, it's equipment that will help there too.
 

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I had this oxidation/darkening problem with most of my beers for a long time. Even ran some experiments to try to test what was going on, couldn't isolate the variable. I believe that hoppier beers are more susceptible, as the acids oxidize fairly easily. There are a few threads on HBT with people having the same complaint and none, so far as I know, have ended in a satisfactory answer.

What fixed it for me? Kegging. I know it's a broken record on here and that the $$ can be daunting for some, but if you can't fix this problem and are committed to brewing it may be your best option. Good luck!
 

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Two possibilities:
1. Stirring in the bottling bucket is aerating the beer.
2. Underfilling the bottles - you mentioned that you recently started filling the bottles fuller. This should help - but even now are you filling liquid all the way to the top before pulling the bottling wand out?
 
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chieftain

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I bottled for the last 8-9 years until I worked into kegging last year. Never noticed any consistent problems...except for hop-centric beers. Had some beers that were fairly pale / delicate like saisons that even 6-8 months later may not have been quite 100% fresh, but still very tasty...but hoppy beers generally seemed to muddy up into the same kind of sticky-sweet hop flavor and darken some in color. One thing that was interesting to me was a handful of bottles from batches would be fine....but the majority of them were so afflicted.


The first beer I kegged was a white IPA. We were over on volume, so we bottled 1gal the same way we normally did (with an exposed bottling bucket, no purging of bottles or anything, etc) and kegged the rest. I didn't have the hardware yet to do a forced transfer into the keg, so I ran some CO2 into the keg with a hose, and gave it a few blasts as it was racking in via siphon as well. The kegged beer ended up great - crisp, bright hop flavor, to where you could pick out different characteristics of different hops. We just opened a bottled version at a recent brewday and did a side-by-side...I tasted the same old sticky-sweet + muted, muddied hop flavor in that one. It appeared a bit darker than the kegged version, though I don't think my buddy had the bottle crashing in the fridge for very long and it wasn't as clear. Pic: https://goo.gl/photos/keSHBnFqhJA4dTHPA


If you don't think you'll end up kegging, you can still get a CO2 tank as you had mused earlier, and one thing I would also throw out for consideration is to get one corny keg and use that as your bottling bucket. You would then have a few options here as to how far you'd want to go to minimize O2 exposure, but they're probably all better than your current process. On the more basic end would be to still dry-hop as you do now, put priming sugar solution in bottom of keg, attempt to do some amount of purging of headspace via CO2, and with the lid on the keg and the relief valve open, rack in through the beer out tube from your fermenter using CO2 to push the beer. Then you could use CO2 + a picnic tap + bottling wand or some similar setup to bottle.


It's an equipment hit (tank, keg, quick disconnects, etc), and CO2 isn't free, but if there's a chance you do want to advance to kegging, it's equipment that will help there too.

thanks, this was very good food for thought, and it's good to hear about your personal comparison of two beers packaged differently. I'm going to wait and see how a recent Double Sunshine clone turns out before making any major changes. I am considering kegging, but it would be via a 2.5 gallon or 3 gallon one, cause I don't have space for a kegerator and I'm the only one drinking this beer...
 
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chieftain

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I had this oxidation/darkening problem with most of my beers for a long time. Even ran some experiments to try to test what was going on, couldn't isolate the variable. I believe that hoppier beers are more susceptible, as the acids oxidize fairly easily. There are a few threads on HBT with people having the same complaint and none, so far as I know, have ended in a satisfactory answer.

What fixed it for me? Kegging. I know it's a broken record on here and that the $$ can be daunting for some, but if you can't fix this problem and are committed to brewing it may be your best option. Good luck!

Thanks, appreciate the feedback. Good to know I'm not alone. I'm going to tweak my bottling process once or twice more before calling it quits and moving to the keg. But it's nice to know that it offers salvation from this really annoying problem.
 
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chieftain

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Two possibilities:
1. Stirring in the bottling bucket is aerating the beer.
2. Underfilling the bottles - you mentioned that you recently started filling the bottles fuller. This should help - but even now are you filling liquid all the way to the top before pulling the bottling wand out?

Yep, I originally was racking my beer to the bottling bucket before adding the priming sugar, and then stirring it in. For the last 2-3 beers, I've switched that order up. Verdict is still out. I was always very careful not to stir it too vigorously though.

My previous method of bottling was to use one of those bottling wands attached to a hose that was attached to the bottling bucket. I would pull the wand out just before the beer reached the top of the bottle (I'm using bombers). For the last beer I bottled, the DS clone, I used a racking clamp and filled the beers higher, allowing it to overflow before withdrawing the tube. With my previous method, I determined I was leaving about 2 inches of headspace. With the racking clamp, I left it closer to .75 inches or so.
 

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With 2" headspace, you might have been filling a little low, but definitely not with 3/4". I really doubt it even 2" was enough air space to cause a problem.
 

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Yes, I would assume fruit beers would be similar- except that adding fruit generally creates some fermentation and perhaps the oxidation risk would be minimized? I'm no expert on that, as I rarely make fruit beers, but I am a winemaker and adding fruit does usually kick off a secondary fermentation.

Darkening is usually one of the first signs of oxidation, actually. Long before flavor changes much, the beer will darken a bit and then start to stale a bit. A bit later on, it will take on "sherry" like flavors or brandy-like notes, or even a hint of metallic flavor in beers with darker roast malts, and when it's much worse is when you get the classic "cardboard" flavors that are most well known. The beer is very far gone by that point, so those "cardboard" flavors aren't as common.

Early oxidation is the most common flaw present in most of the beers I judge in competition, but many brewers who don't know the classic early signs don't know that. I think they are looking for "wet cardboard", and not early staling type of reactions and flavors.



Thank you for the reply Yooper.



I found a older picture of the IPA in question, so I thought I would post a then and now comparison of the beer. Check it.


Then. This was how the beer looked from the keg.

20151202_140502_zpsw7vaj4jy.jpg





After bottling, the same beer a few weeks later (this past weekend to be exact).

Zombi%20Nazi%20IPA%204-2-16_zps4brsoelm.jpg



The beer doesn't seem to have the same flavor and aroma as it did when pulling from the keg. I also have some others still bottled I'm going to look into. If those show some of the same signs, then I'll have to re-evaluate how I've been bottling my beer. Fingers crossed............
 

blizz81

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Cripes! I know the lighting is different, but that's still quite a significant difference in color.
 

Yesfan

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Cripes! I know the lighting is different, but that's still quite a significant difference in color.


The first pic was taken 12-04-15. The second was 4-2-16. This was an IPA I brewed around Thanksgiving. I kegged it and when it was close to being half gone, I bottled a 12 pack to put away to make room for the next keg once this one kicked.

The color never changed while pulling from the keg, but the bottles are a different story. Is there a possibility that some of the other bottles won't be oxidized, or will they all be the same? I use a counter pressure filler when bottling from the keg (the infamous Biermuncher beer gun mod).



If I come across a bottle that hasn't oxidized, I'll post another pic for comparison if you all want me to.
 

Rcbandl

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Oxidation generally takes alot longer that a couple weeks to develop. I am going to make a guess that possibly its skunking thats occurring. Do you ferment with the carboy exposed to light?
 

Yesfan

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Oxidation generally takes alot longer that a couple weeks to develop. I am going to make a guess that possibly its skunking thats occurring. Do you ferment with the carboy exposed to light?



Is that directed to me?


If so, no. I have a temp controlled freezer I use. I fermented in the low 60s with this beer and kegged it around Thanksgiving. The time between the two pictures is about 4 months.
 

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