JMS Spirits

Sediment / Cloudiness in Spirit

12 posts in this topic

I'm working on some formulations for a new product using pre-distilled 190pf base spirit, then adding water, sugar, and a few flavor components. I'm using RO water and have confirmed that the flavors are completely water soluble. At some point after blending (typically a few weeks) I've noticed that a white sediment-looking formation collects at the bottom of the bottle. When it is disrupted it "floats" upwards and disperses throughout the bottle, looking similar to rising smoke. When you shake the bottle heavily, it disperses completely but only to return within a day or so. 

I've confirmed that the issue is not caused by any type of bacteria, calcium in the water, or other potentially obvious things. I initially thought cold temperature was the driver, but I've tried putting it in the freezer and it doesn't seem to directly cause the issue. Has anyone ever encountered this before, or do you have any insight into what might be causing it and how to eliminate it? 

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It'd guess minerals in the water.  Do you have a TDS meter? Are you using an ion exchange column after your RO system?

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Probably either minerals (your RO system not working well) or your water soluble ingredients fall out of suspension in the alcohol/water solution.

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@IndySpirits thanks for the response and yes to both, so I've been thinking more and more that it's something besides just minerals in the water. 

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I would think it is the added flavour components are NOT completly completely soluble in your mix. For interest carefully pour some of the clear liquid off the top of a bottle with sediment. Replace with some neutral and see if the sediment dissolves.

Also try leaving out one flavour ingredient at a time to see if one is causing the problem.

If you are happy with the taste of your product then leave to settle out the sediment for a few weeks before filtering and bottling. 

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So we are having a similar issue with our bourbon. We released several batches of bourbon with no issue but in the more recent bottlings, we are getting a post bottling sediment/cloudiness on the bottom of the bottles. Details (feel free to ask more):

Product: Whiskey (fairly standard grain bill), aged in new charred, aged 1 to 2 years.
Water: We use filtered city water through large carbon block for our process water and we run that filtered water through a RO/DI system for our proofing down water.
Filters: We used cartridge filters and run a 5 micron and 1 micron in series.

We had no issues for a long time and then in the last several months we have had this issue. We had thought the issue may be that our RO/DI filters were too old so we swapped them out. That seemed to work on a malt whiskey we released but the most recent bottling of bourbon has the same issue.

Timing: the whiskey looks perfectly clear during and post-bottling. The haze is like a stringy cloudiness on the bottom of the bottle that clears out when shaked.

Any thoughts? We have a 1/2 micron filter we can try but I am skeptical that will fix it. We already filter through a 1 micron which should be more than enough. We also waited a few days between proofing down and bottling so anything that formed should have been filtered out (unless perphaps the agitation of the bottling process hides it).

TIA

 

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Very good chance it is flocking (crystals forming) after it is bottled.

What ABV are you reducing to? Typically, but not necessarily, under 45% you will get flocking.

A few days is not normally long enough for the crystals to grow large enough to be able to be filtered out.

I presume you are not chill filtering. Crystals will grow a lot faster at colder temperatures.

Distillers in this part of the world typically leave diluted spirits about 6 weeks before filtering and bottling.

If you don't like the idea of chill filtering because of the apparent loss of flavor, a compromise is to chill for a couple of days then allow to warm up to ambient for another couple of days. Crystals will form and maybe "steal" too much of your flavor, but as it warms up again some of those crystals will re-dissolve and you should end up with approximately non-chill filtered.

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We do not currently chill filter. We are reducing from 125 proof to 90 proof with RO/DI water.

We could conceivable rest longer before filtering, although that would not be easy with our current set up. My other concern would be that when the bottles are shaken or moved, the cloudiness/sediment seems to mix back in so I'm not confident one way or the other that filtering after resting would cure the issue although it is worth a try.

Any idea on why this would be happening now? We are essentially making the same product, in the same space, using the same ingredients, aging in the same conditions (albeit a little longer) and didn't have this issue for the first year or two of operations. The only thing I could think of was that our filters were getting old (although I believe the RO/DI system was showing a read out of zero on the output but we changed the filters in it regardless.

I don't think it is an issue with our process (ferment, etc) because we didn't have the issue before and had it with a beer we distilled into an aged whiskey from a brewery in our same building.

 

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@JMS Spirits are you rinsing your bottles with spirit before filling? Ive encountered a problem like this before in which there was residue in the glass bottles from manufacturing that upon filling those bottles a sediment appeared at the bottom a few days after.

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This is likely flocculation. The source is likely the barrel in the case of the bourbon. We see this, depending on size, type, char, and source of the barrel, length of aging, etc. Most of this appears to be due to oligosaccharides. They affect mouthfeel and sweetness. You can chill filter them out, but it will change the flavor profile of your spirit. You did not say if there was ANY change in the aging process between older and newer batches of bourbon. We get this in some of our whiskies, and we educate our customers about it, you might have to do to the same. To eliminate it, chill filter.

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UPDATE:

Thanks for all the replies. We *think* we fixed this. We still can't isolate what caused this but it appeared to form over a week or so. We dumped the bottles out, let it settle and filtered through 1 micron and .5 micron (not chill) and the filters did appear to pull out the flocking or whatever we can call it. We rebottled and it looks great. Moving forward, we will probably dilute down to bottling proof more slowly and tank and then filter before bottling and go from there. Will update again if we have the same issue.

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