D47 Cider late developing sulphur

[hahayepyep]

I went to check a bulk-aging cider (6 months from pitch) to find a strong rotten egg sulphur smell had developed. I've not encountered this occurring so late before. There are no other signs that scream contamination, so I'm not so sure it's spoilage from an organism. I've had this smell during primary before, but it always subsides. This is my first attempt using D47 for a cider, but I haven't heard of this being a trait of it.

I have a little experience making ciders and have never encountered this particular problem before. In fact, time usually seems to help with sulphur problems in the past. I'm hoping someone here can help me sort this out. I'd really like to know where I went wrong here and, ideally, save this batch.

PROCESS:
I started the ~5 gallon batch October 23, 2017. Recipe is as follows:

In 6.5 PET BMB:

• 5.5 gallons fresh, unfiltered, pasteurized orchard cider.
• 2.5 tsp pectinase (thought I had more on hand, used what I had)
• (pectinase allowed 12 hrs to work)
• 1 tsp FT Blanc Soft (tannins)
• 1.25 tsp Booster Blanc (nutrient)
• 1 pkg D-47 (rehydrated with Go-Ferm)
• 0.5 tsp Fermaid O (added at 72 hrs)

Fermenter was kept at 62F (with a +/- 2F appx swing each way).

• Day 2 strong signs of fermentation.
• Day 7 ferment had slowed substantially.
• Day 14 much of the yeast had fallen.
• Day 30 racked to 5 gallon carboy.

The taste sample from day 30 was good considering age. The only faults I found were consistent with green dry cider / white wine.

The cider sat undisturbed aside from airlock top-up in a ~64F basement until April 23 (6 months from pitch). I intended to bottle that day, but when I pulled the cover, I got a strong whiff of rotten egg.

Shooting from the hip, I racked to another 5 gallon carboy to see if it drove off the smell. I had a sulphur problem with a much younger cider once. After reading that introducing the cider to copper might remediate the sulphur smell, I made a little copper tubing apparatus that I fit on the end of my siphon hose to pass the batch through the copper. It seemed to work that time, so I tried it again.

A week later, no change, so I tried it again. Another week later, no change.

Next I tried adding campden tablets and 1tsp of ascorbic acid. After a 3rd rack through the copper tubing, there seems to be LESS rotten egg smell, but I still catch much more than I would like.

So, what now? The advice I've gotten so far is: "wait longer", "dump it", and (the one I'm most curious about) introduce fresh yeast and more sugars to see if restarting the ferment could get the yeast to clean up.

Any help?

(edited for omissions/corrections)

 

[kl Roosevelt brewer]

Did you D gas your batch during fermentation on a daily basis?

 

[hahayepyep]

Yes. Forgot that in the process. For the first 5 days, I remove the lid and replace it with a "flour sack" towel and rubber band. I swirl the cider vigorously until no more foaming occurs.

 

[kl Roosevelt brewer]

I have had really good luck with d47. I use it in my Mead and I'm also using it in my maple syrup wine. One thing I learned is when you transfer from your bucket into your glass carboy take everything even the trub. And then for the next month or 6 weeks keep stirring and agitating the trub up into your batch and eventually the particles get heavy enough and it clears almost instantly then rack into your long-term storage keg or glass carboy

 

[Maylar]

This is really odd. I've had sulfur in the first stages of primary from lack of nutrients, but never after aging. Only thing I can think of is if you sulfited the must when you racked it and accidentally overdosed the k-meta.

 

[hahayepyep]

This is really odd. I've had sulfur in the first stages of primary from lack of nutrients, but never after aging. Only thing I can think of is if you sulfited the must when you racked it and accidentally overdosed the k-meta.

At the transfer to secondary (30 days) I used 3 campden tablets (I use the LD Carlson 550mg Potassium ones). That's never caused a problem for me before.

I'm stumped.

 

[kl Roosevelt brewer]

let me ask a stupid question. Isn't Camden tablets basically sulfur?

 

[hahayepyep]

Yep, but in the form of SO2 (which smells like a struck match). That's not the problem smell. What I'm getting is rotten egg smell--I assume H2S.

 

[kl Roosevelt brewer]

Sorry man I guess I am no help I have never had an experience in 10 years that anything's smelled like sulfur

 

[hahayepyep]

I wonder if I need to pay more attention to the possibility of a spoilage organism of some sort.

 

[kl Roosevelt brewer]

Did you use campden tablets in your fresh juice before you even got started?

 

[hahayepyep]

Yes. Yet another detail I forgot in the OP. 5 tablets the day before the pectinase. I can't remember where I picked up the habit, but I've always followed a 1 tablet per gallon in the juice 12-24 hrs before pitching (or pectinase) and half that again when racking. The tablets don't split well and my 5 gallon batches are always fat, so I just use 3 on 5 gallon batches.

I've been told over-and-over that it's not strictly necessary with pasteurized juice, but when I use pectinase on unfiltered juice, I don't like the idea of letting it sit so long having been exposed to my basement air without it. I don't use it on clear pasteurized Treetop-type juice because I pitch right away with that.

ETA: Thanks for all the help, btw!

 

[kl Roosevelt brewer]

When you speak of a basement a person can imagine something dark and dank and musty and foul-smelling or picture a pool table with sheetrock on the walls. What kind of basement do you have?

 

[hahayepyep]

Ha! Finished basement (sans pool table) with the exception of the mechanical room. The entire level is climate and humidity controlled. It's a 100 year old house, so it'll never be sterile, but it's pretty clean.

To be fair, I have only ever had two batches of anything spoil. One was after an airlock went dry and was forgotten about leaving a pumpkin ale open to the elements and the other was when I was brand new at all this and naively used wild fruit in a mead.

I don't see any signs that lead me to think it's an obvious case of easy to identify contamination: no pellicle, no scum, no film, etc.

 

[kl Roosevelt brewer]

Well there's always the last resort which is to pull out your little still and salvaged the alcohol out of it

 

[kl Roosevelt brewer]

I made a batch of cherry wine using pie cherries and left the pits in. I ran the whole batch through my little still

 

[kl Roosevelt brewer]

That was back in the very early 80s and late 70s when the woods got shut down here in the Northwest over the spotted owl controversy and money was real tight

 

[johnnyseko]

Yes. Yet another detail I forgot in the OP. 5 tablets the day before the pectinase. I can't remember where I picked up the habit, but I've always followed a 1 tablet per gallon in the juice 12-24 hrs before pitching (or pectinase) and half that again when racking.

The only time I've had a sulfur problem (once, so far) was the one and only time I added campden tablets prior to pitching. In hindsight I should have followed up with nutrients. This occurred with 3 different yeasts when I was testing different strains (wyeast 1450, S33, and WLP028) in single gallon batches. The Cotes des Blanc from another gallon was the only one that didn't have a big issue. These batches went straight from primary to bottle - mistake on my part - I was in a hurry and wasn't thinking.

Not sure why yours won't dissipate. My bottled batches kept it sealed up unfortunately. I've tried pouring it and letting it sit in the glass for a while before drinking but it won't go away. I considered getting a copper scouring pad to pour it through but never got around to it.

 

[Yooper]

The only thing that I can think of is perhaps it sat on lees for a long time? I generally rack after 60 days if there are any lees, as some yeast strains get a bit foul when left as lees for a lengthy time.

 

[hahayepyep]

The only thing that I can think of is perhaps it sat on lees for a long time? I generally rack after 60 days if there are any lees, as some yeast strains get a bit foul when left as lees for a lengthy time.

I'm wondering about this also. I likely should have gotten it off that yeast.

Think it might help to start the ferment back up so the yeast can get a crack at cleaning up?

I just went and checked the carboy. It now smells like apple wine with some sulphur, whereas before the ascorbic acid / copper tubing treatment, it smelled of nothing but a rotten egg mess. Since there seems to be some effectiveness with this treatment I'm wondering if a) it simply needs more time to dissipate, b) the dosage of ascorbic acid was insufficient, c) the surface area and/or contact time of the copper tubing was insufficient.

I think I'll let it sit a week and go from there.

 

[Maylar]

When I've had H2S in primary, stirring the cider a couple times a day helps it to dissipate. But at that level, there's CO2 bubbling and oxidation isn't a big concern. Where you're at neither is true.

Can you keg it? Pressurizing through the liquid side of a keg and purging can make a lot of difference.

 

[Yooper]

I'm wondering about this also. I likely should have gotten it off that yeast.

Think it might help to start the ferment back up so the yeast can get a crack at cleaning up?

I just went and checked the carboy. It now smells like apple wine with some sulphur, whereas before the ascorbic acid / copper tubing treatment, it smelled of nothing but a rotten egg mess. Since there seems to be some effectiveness with this treatment I'm wondering if a) it simply needs more time to dissipate, b) the dosage of ascorbic acid was insufficient, c) the surface area and/or contact time of the copper tubing was insufficient.

I think I'll let it sit a week and go from there.

No, yeast won't clean up issues from autolysis or stressed yeast. If it's improving, that's good. I dose with sulfites at 50 ppm and then splash rack, and see if that helps dissipate more of it.

If that doesn't help, Jack Keller's excellent site has this advice:

There are several causes of H2S formation.

• Too much elemental sulfur, usually from grapes or other fruit that were dusted with too much sulfur during the growing season.
• Lack of appropriate and sufficient nutrients (nitrogen, yeast hulls) before and during fermentation
• Bacterial contamination due to inadequate sanitation

Books, bloggers and discussion forum participants have written for years that Montrachet yeast promotes the formation of H2S, but in all my many years of using this yeast, one of my favorites I might add, I have never developed H2S while using it. I think everyone is perpetuating an urban legend of winemaking. I have certainly used it hundreds of times without even a sniff of H2S.

Okay, if you know the causes of H2S formation, then you can deduce how to prevent it. Simple logic. But that does not help our friend who already has it. So, what to do?

I asked him if he has tasted the must since he detected the smell? I am curious as to what he reports, as I once (and only once) tasted an H2S infestation and have an idea what he should report if he had done so. I'm really just curious. More importantly, I asked what yeast strain did he use? If he followed my recipe, he used Montrachet, but if he used another then I can advise him on nitrogen requirements, if any.

First, do add nutrients. One teaspoon per gallon should be adequate foe most yeasts, but not all. The nutrients can be dissolved in a little must and stirred in. All fruit musts need nutrients and, depending on the yeast strain, that might apply to grapes, too.

Second, if he has an SO2 test kit, measure the amount of free (unbound) sulfur in the must. If under 50 ppm, add just enough potassium metabisulfite to bring the free SO2 level up to 50 ppm.

Third, rack the must into a sanitized carboy and let it splash a lot in the process. You want to introduce O2 into the must.

Fourth, attach the airlock and wait a few hours. Then remove the airlock and smell it again. If the smell is still prevalent as more than a trace, rack it again as before, affix the airlock, and head for a hardware store, Home Depot or similar store and buy a 1-foot piece of 3/8 to 1/2 inch copper pipe (tubing). Have them cut it into three 4-inch pieces. At home, run a 4-foot piece of sturdy string through one piece of tubing and loop it around and tie it to the string going into the tubing. Adjust the string so the tubing hangs straight up and down and is snug. Run the string through the other two pieces of tubing so all 3 hang straight. Place the tubing and string in a glass bowl and cover with 10% sulfite solution for 2-3 minutes. Remove, rinse with distilled water, drop the tubing into the carboy and swing it around for about 2 minutes. Remove the tubing and rack the must again. Affix the airlock and wait one hour. Smell the must. The smell should be reduced.

Fifth, if the smell is still strong, place a large funnel in a sanitized carboy, hang the copper tubing pieces through the funnel and suspend them a few inches below the funnel. Slowly pour the must through the funnel and into the carboy. It will cascade over the copper on the way in. Remove tubing and funnel, affix the airlock and wait it out. When the must finishes fermenting, fine it with gelatin fining agent per the manufacturer's instructions and rack. Let it clear and rack again.

Another method of copper treatment is go to the supermarket and look in the housewares section for a copper scrubby. (These are less common than they used to be and I once visited four supermarket chains before I found one. I bought three and stored them in baggies just in case.) At home, sanitize it with 10% sulfite solution for 2-3 minutes, rinse with distilled water, and squash it down into a large funnel placed in the mouth of a sanitized carboy. Slowly pour the must through the funnel into the carboy. Repeat in an hour if needed. When the must finishes fermenting, fine it with a gelatin fining agent per the manufacturer's instructions and continue as above.

Of all the things that can happen to a wine, H2S is the most frustrating but certainly not the worse. All those that are worse have no cure, so you just dump the wine. H2S is frustrating because it can be cured, but takes some effort. Worse still, about one in four times it is too far gone when discovered to correct.

I know many of you out there will say, "Why not just treat with copper sulfate and be done with it?" Here is my rule. I do not publish recipes for wine from plants I know to be very poisonous or toxic, and I do not publish cures to wine problems that require adding a poisonous substance. Copper sulfate is very poisonous. If you cannot measure a substance to hundredths of a gram and liquids to a fraction of a milliliter, don't go there. I don't play Russian Roulette and would never ask you to. Use one of the more labor intensive but safer methods above.

Most people who get H2S will get it post-fermentation. Adjust the instructions above to suit the timing.

 

[hahayepyep]

...Can you keg it? Pressurizing through the liquid side of a keg and purging can make a lot of difference.

I don't keg right now, but have been slowly acquiring the bits. I have CO2 tanks, regulator, hoses, fittings, etc that I've been snagging when I find a deal. Planning to get everything in place by this fall and basically just need the fridge/freezer to dedicate to it and the kegs. Maybe I'll speed up the keg acquisition.

 

[kl Roosevelt brewer]

I have totally gotten away from the wine bottle thing and gone strictly 2 kegs. My problem is I don't have a place cool enough to store my kegs. So back in March I got a guy with an escavator up here and dug me a hole and buried a 2-foot pipe straight up and down 7 feet deep. It's got a bolt on lid plus an extra wooden box lid with r21 solid insulation that goes over the top. Back in March I put a probe 2 feet off the bottom and it was 42 degrees now it's up to 49 degrees. It holds four kegs 5 gallon kegs per layer and it will hold three layers which is 12 kegs. It is my geothermal electricity free refrigerator

 

[hahayepyep]

No, yeast won't clean up issues from autolysis or stressed yeast...

Thanks, I'll quit chasing that rabbit, then.

 

[hahayepyep]

I have totally gotten away from the wine bottle thing and gone strictly 2 kegs. My problem is I don't have a place cool enough to store my kegs. So back in March I got a guy with an escavator up here and dug me a hole and buried a 2-foot pipe straight up and down 7 feet deep. It's got a bolt on lid plus an extra wooden box lid with r21 solid insulation that goes over the top. Back in March I put a probe 2 feet off the bottom and it was 42 degrees now it's up to 49 degrees. It holds four kegs 5 gallon kegs per layer and it will hold three layers which is 12 kegs. It is my geothermal electricity free refrigerator

That's quite the cellar!

 

[kl Roosevelt brewer]

By the time I bought the pipe in the lid built the box and paid the guy to dig the hole it was about 350 bucks

 

[kl Roosevelt brewer]

I live on a mountain with coarse sand and Rubble Rock so there is no standing water but I do get quite a bit of condensation in there because it's just sand on the bottom. I figured just stainless steel kegs aren't going to get hurt staying in there a year or two

 

[hahayepyep]

I racked again today through the copper tubing and there's definitely some improvement. Now I'd characterize it as "I'm picking up a little sulphur in there" rather than the stink bomb it was before. So, I think it's not a sewer pour just yet. I'd like to get it in bottles and end all this handling of it, but I don't imagine the sulphur will age out once bottled. Given the incremental progress, I'm tempted to rack with the copper once more and then bottle.

The only thing that I can think of is perhaps it sat on lees for a long time? I generally rack after 60 days if there are any lees, as some yeast strains get a bit foul when left as lees for a lengthy time.

I had a chance to run this case by someone with a microbio background and significant winemaking experience over the weekend. He went straight for this idea, too, and was pretty confident that it was the result of my lazy racking approach and bulk again on the lees.

 

[Yooper]

I racked again today through the copper tubing and there's definitely some improvement. Now I'd characterize it as "I'm picking up a little sulphur in there" rather than the stink bomb it was before. So, I think it's not a sewer pour just yet. I'd like to get it in bottles and end all this handling of it, but I don't imagine the sulphur will age out once bottled. Given the incremental progress, I'm tempted to rack with the copper once more and then bottle.



I had a chance to run this case by someone with a microbio background and significant winemaking experience over the weekend. He went straight for this idea, too, and was pretty confident that it was the result of my lazy racking approach and bulk again on the lees.

Some wine yeast strains are much better for aging on lees than others. There is a technique called sur lie, in which some wine is aged on the lees (with a good yeast strain), but even then the lees are stirred at intervals to help prevent autolysis.

If you can sulfite and splash rack once more, you may not need the copper treatment. I would try that next, to see if that gets rid of the rest of the sulfur. If not, you can always give it the copper treatment.

You're correct that you dont' want to bottle it until it's gone- it won't dissipate in the bottle and it may very well get worse.

 

[hahayepyep]

The tech data sheet for D47 suggested extended lees contact could be beneficial and that it was a low H2S producer. That's why I gave myself licence to go somewhat laissez faire. Clearly, my technique is the culprit, here, and I can't blame the tools. I'll take better care with the next batch.

I took a small sample before racking, swirled it vigorously in a wine glass, and chilled it. Sulphur was minimal, so I think a splash rack may just do it. I have to say that I'm very happy with the flavor. It's certainly more complex than the ale yeast batch I made with the same juice. The tannin addition in this batch likely takes part in that, too, but it's hard to tell they were ever the same apples. There's a light peppery/spicy thing going on that I assume is a positive result of the extended yeast contact. In the next D47 batch I try I'll be aiming to get that flavor profile again but without the stench.

 

[hahayepyep]

Also, thanks for the help, Yooper! It's nice to have some guidance as I work my way through knowing just enough to be dangerous.