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Another Thread about Sulfides etc.

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Angelic Alchemist

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Sep 14, 2009
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Houston, TX
www.angelic-alchemy.com
01/03/10:
~1+ gallon Autumn Wildflower honey from my buddy, Kerry
4 Gallons Spring Water (Ozarka)
10g (2 packets) K1V yeast, rehydrated in warm water
OG = 1.09 (planning to go dry, ~12%pABV)
T = 72F degrees

Added 5T Super Ferment post lag (~14 hours later)

01/05/03: pH ~3.0, added 1tK2CO3 to raise pH to 3.6, SpG = 1.09
01/06/10: Noticed sulfur egg smell, added 2.5T super ferment
01/08/10: SpG = 1.01, still stinky
01/13/10: still stinky, added 1 capsule of yeast hulls and 1g Epsom Salts
01/15/10: SpG = 1.005, splash racked off gross lees, stink stank stunk
01/23/10: Even more stinky, rubber tire smell

Okay, so how many pre-1982 pennies should I use, and how much vitamin C? Also, I'm really interested as to what the heck I did wrong that would stress out K1V. I've never had this problem with this strain of yeast before.
 
The vitamin C is usually 25 ppm (25 mg/L). This mead is young so you probably don't have too many disulfides that would require the vitamin C, but hey, it's good for you right?

A clean copper scrub pad from the grocery store works pretty well. You can tie a little string or dental floss to it, and drop it in. Then you can pull it out in a little while without problems.

A good dose of yeast hulls might also bind up some of the odor causing stuff.

It is a little unusual for K1V to become so stinky.
 
I had a really bad first experience with that yeast, lots of sulphur smells, and I thought I'd even given it a half decent amount of nutrients, especially for a "low" nutrient needs yeast... next time I'll be more careful with it I guess, treat it like a higher needs yeast.
 
Angelic Alchemist said:
01/03/10:
~1+ gallon Autumn Wildflower honey from my buddy, Kerry
4 Gallons Spring Water (Ozarka)
10g (2 packets) K1V yeast, rehydrated in warm water
OG = 1.09 (planning to go dry, ~12%pABV)
T = 72F degrees

Added 5T Super Ferment post lag (~14 hours later)

01/05/03: pH ~3.0, added 1tK2CO3 to raise pH to 3.6, SpG = 1.09
01/06/10: Noticed sulfur egg smell, added 2.5T super ferment
01/08/10: SpG = 1.01, still stinky
01/13/10: still stinky, added 1 capsule of yeast hulls and 1g Epsom Salts
01/15/10: SpG = 1.005, splash racked off gross lees, stink stank stunk
01/23/10: Even more stinky, rubber tire smell

Okay, so how many pre-1982 pennies should I use, and how much vitamin C? Also, I'm really interested as to what the heck I did wrong that would stress out K1V. I've never had this problem with this strain of yeast before.
Click to expand...

Hiya AA,

Do you have any more of that honey left? If so, would you do me a favor and take about a half a cup and heat it slowly, then give it a whiff. Let me know if you get any out of character aromas from it.

Cheers,

Oskaar
 
Oskaar said:
Hiya AA,

Do you have any more of that honey left? If so, would you do me a favor and take about a half a cup and heat it slowly, then give it a whiff. Let me know if you get any out of character aromas from it.

Cheers,

Oskaar
Click to expand...

I don't have any on hand, but Kerry has >50lbs of the stuff at his place. Another one of my friends recently passed his sommelier exam and has a far superior palate to mine. I'll get his opinion on it. Odd thing is, I used the same honey in a 1 gallon sweet mead batch and it's running fine. No off aromas at all.
 
I threw 1500mg vitamin C + a cleaned 1974 penny into the must and the smell is less, but not gone. Medsen, I just haven't made it to the grocery store yet but plan on doing so in the near future for that mesh sponge. Pete, I should also be going over to Kerry's this weekend to get some honey, though I'm currently not speaking to the guy with the palate (what is it with me butting heads with people I like?). That's okay, my nose works fine. Will f/u.
 
Angel,

It is important to know that while the reaction between mercaptans and copper is pretty quick, the transformation of disulfides back into mercaptans (the purpose of the ascorbic acid) will take some time - often weeks to a couple of months. The other thing worth noting is that if there is any fermentation still going on, some yeasts actually throw MORE H2S in the presence of copper, so the penny treatment is not a good idea until you are sure that all the yeast have finished doing their thing.

Now since you don't want too much copper in your mead, you probably want to allow the Vit-C to do its work for a week or two with the penny removed, and then add it back in for a day or so. If that doesn't clear the rest of the stink, pull the penny out for another couple of weeks, let the C continue to work its magic, and repeat. Do that as many times as it takes to clear the stench, or until you've lost patience completely with it. Sometimes (but thank goodness rarely) even copper treatments don't completely clear sulfurous odors, no matter how hard you try.
 
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Oskaar said:
Hiya AA,

Do you have any more of that honey left? If so, would you do me a favor and take about a half a cup and heat it slowly, then give it a whiff. Let me know if you get any out of character aromas from it.

Cheers,

Oskaar
Click to expand...

Okay! Sorry about the delays. I got some more of that honey and heated it, and it smells...weird. I can't really put my finger on the aroma. It's not foul, just unusual. The closest thing I could think of when I smelled it was stone ground corn tortillas. A little mineral smell and a little nutty/vegetal smell.

In other news, I've splash racked the batch a few times and the smell has faded, but it is still there.
 
Update! Per the advice from this thread, I removed the penny from the must and splash racked the remainder of the 5 gallon batch that had already been treated with Vitamin C. I let this sit for about 2 weeks. Then I splash racked it again (it was reduced to 4 gallons at this point) to a 3-gal carboy and a 1-gal carboy. Smell still present, but not like rubber tires anymore. It was back to the egg smell. I added a single, clean, copper penny to each one (I don't remember the years from the pennies, but they were old) and allowed them to sit for a few days. I splash racked both carboys this weekend and the odor is completely gone. The musts smell of honey. I noticed the carboys still stank a bit, so I sanitized them thoroughly before transfering my must back into them.

Take home message: a single copper penny will scrub the sulfur smell out of 1 gallon or 3 gallons, after a few week's treatment with vitamin C and splash racking.
 
Beautiful! You have witnessed (or smelled) firsthand the conversion of diethyl disulfide back to mercaptans, and then the chemical binding and neutralization by copper!!

FWIW, the small amount of copper that reacts with the mercaptans will form an insoluble chemical, copper sulfide, that will precipitate out. So will any stray yeast cells. You will want to carefully rack, leaving any noticeable sediment behind, before bottling since the reductive potential provided by autolyzing yeast can actually reverse the copper reaction, releasing those mercaptans and allowing metallic copper ions to go back into solution in your mead. Not a good thing for long term storage. ;)
 
wayneb said:
Beautiful! You have witnessed (or smelled) firsthand the conversion of diethyl disulfide back to mercaptans, and then the chemical binding and neutralization by copper!!

FWIW, the small amount of copper that reacts with the mercaptans will form an insoluble chemical, copper sulfide, that will precipitate out. So will any stray yeast cells. You will want to carefully rack, leaving any noticeable sediment behind, before bottling since the reductive potential provided by autolyzing yeast can actually reverse the copper reaction, releasing those mercaptans and allowing metallic copper ions to go back into solution in your mead. Not a good thing for long term storage. ;)
Click to expand...

Yeesh. I didn't think this simple batch would turn into such a pain. I was hoping to carbonate it. Should I let it clear, rack and repitch with priming sugar? Is sur lees aging a bad idea because of this phenomenon? I wanted to just forget about that carboy for a year.

Also, fingers crossed that it's not oxidized to Hades from all the splash racking. :p
 
What I would do:

Let it clear, or at least let it "settle" for 2 to 4 weeks, and then carefully rack into a different container. All of the copper sulfide will have settled out, and almost no autolysis will have occurred in that short of an interval.

Once you have removed the majority of the copper sulfide you can let the rest age sur-lie to your heart's content, or prime with some fermentable and maybe an additional amount of yeast (just to be sure of some viable cells) before you bottle. ;D

And Medsen beat me to it, again! I've gotta learn to type faster!! ;) (But I don't think you need to resort to filtering, once the copper sulfide is definitely out of there.)
 
wayneb said:
What I would do:

Let it clear, or at least let it "settle" for 2 to 4 weeks, and then carefully rack into a different container. All of the copper sulfide will have settled out, and almost no autolysis will have occurred in that short of an interval.
Click to expand...

Hmm. My musts almost never clear that quickly. Will a clarifying agent be okay to use at this point, or will it do something funky with the copper compounds? I have some bentonite clay and sparkloid on hand, but prefer using Super Kleer when the LHBS has it in stock - it's fast and easy to use.
 
Yup. It will work. The copper sulfide is basically inert unless it gets electrochemically pulled apart, so adding any common fining agent won't affect it, and that will help pull the yeast out. Within 2 weeks of time though, all the copper sulfide will have settled out. As Medsen suggests, the yeast remaining in there are chemically compromised (since they gave rise to the stink initially), so there is a chance for some H2S production out of them whenever you introduce more sugar.

He is a little more worried about it than I would be... but in this case there's no harm in a more conservative approach.
 
wayneb said:
Yup. It will work. The copper sulfide is basically inert unless it gets electrochemically pulled apart, so adding any common fining agent won't affect it, and that will help pull the yeast out. Within 2 weeks of time though, all the copper sulfide will have settled out. As Medsen suggests, the yeast remaining in there are chemically compromised (since they gave rise to the stink initially), so there is a chance for some H2S production out of them whenever you introduce more sugar.

He is a little more worried about it than I would be... but in this case there's no harm in a more conservative approach.
Click to expand...

Yeah, I'm in no mood to continue struggling with this batch. My buddy Kerry gifted the honey to me from his apiary and I was almost crying over it when it went south. I'll add a fining agent to it tonight and rack it when it clears completely. Dang, that means I need to go buy champagne bottles in a few weeks. I guess I should forget about treating myself to that refractometer for now. :mad:
 
Angelic Alchemist said:
Dang, that means I need to go buy champagne bottles in a few weeks. I guess I should forget about treating myself to that refractometer for now. :mad:
Click to expand...

Bah!
Think Wedding Crashers.

You just need to go to a wedding. While everyone else is fighting over the centerpieces, you can cart off all the Champagne bottles (though getting those labels off can be a pain - they are usually designed to stay on in an ice bucket)
 
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