Ultrasonic Lab Trials

[Badger]

(Note: this was originally posted in the Nuclear thread but I'm starting a new thread here)

Hi there, Badger here.

There has been quite a bit of discussion about the “nuclear process” and many many pages of anecdotal experiences, mostly positive. I was interested in acquiring some objective data to complement what has already been posted. I recently visited a local distillery where the head distiller is a complete chemistry geek (MSU Distilling Program grad student, thesis on barrel aging, etc). I reached out to him on this topic and was pleasantly surprised when he agreed to run samples through his lab and gas spectrometer. Below, please find our emails and in the next post, I’ll present my initial thoughts on possible trials.

(Note: I’ve redacted names from the emails to keep his distillery from appearing to approve of home distilling)



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On Tue, Apr 30, 2013 at 1:13 PM, BADGER wrote:
Dear Xxxxx,
My name is BADGER and we talked the night that the Homebrewers Guild took a tour of the distillery. I was the “home enthusiast” who discussed with you whether it was possible to hit azeotrope with something other than a 30+plate still. You challenged me to bring in a sample of a suspected azeotrope to put through your lab. While I don’t have that, I do have another topic that might interest you.

Currently, several of the online forums who geek out on this kind of thing are discussing the use of either microwave or ultrasonic cleaning to “smooth” or speed up/improve aging (some are doing it just to distillate while some are using wood chips, etc). While no distillery that I’m aware of uses microwaves to improve their spirit, there are at least a couple that seem to be using a version of ultrasonic cleaning. While there is general agreement that these processes improve taste, there was some question as to whether there is an actual quantifiable chemical effect taking place and, if so, what that is. Unfortunately, we don’t have access to the kind of lab you use every day.

If, and only if, the results of such an experiment would interest you (I think I remember you saying you did your thesis on aging), I’m wondering if you’d be willing to put several identical samples (untreated, microwave treatment, ultrasonic treatment, for instance) through your lab to see a side-by-side chemical comparison of the various treatments.

I realize this is fairly brazen of me and you are a very busy person. I’ll completely understand if, for any number of reasons, you aren’t interested. However, I figured it never hurts to ask. You seemed very open-minded about being creative with the art of distilling and I thought that, just maybe, this would appeal to your own inner geek. 

In any case, thanks again for a fun and informative tour. I can’t wait to see all the fun things that come out of [Xxxxxx Distillery] in the coming years.

Sincerely,
BADGER
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On May 10, 2013, at 5:46 PM, "XXXXXX wrote:
Hi BADGER,

Sorry for the delay and what will probably be a short response. I am totally interested in this. I would love to run samples and right now we are setting up our GC with the help of Kara Hulce, who was also on the tour. She is our new lab intern and I think we should absolutely run these samples.

I am aware of Terressentia and their ultrasound process. They asked me to help validate their work and I took a look at their website and declined. I can think of at least two or three improvements that are possible and we shall examine them.
Start pulling your samples together and let us know when you might be ready to run them.
Best,
XXXXXX

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On Sat, May 11, 2013 at 10:25 PM, BADGER wrote:
That is great. Thanks so much!

I'll contact some people about getting the samples. In the meantime, what kind of parameters are we talking? Sample size? Are there certain protocols that need to be observed to avoid contaminated or otherwise compromised results? How many samples (I have no idea if the process is 5 min or 5 hours) are realistic?

My initial idea would be something like 8 samples:
1. control white spirit
2. microwaved white spirit (minor dose)
3. microwaved white spirit (major dose)
4. ultrasounded white spirit (minor dose or low power)
5. ultrasounded white spirit (major dose or high power)
6. white spirit microwaved with oak
7. white spirit ultrasounded with oak.
8. white spirit "traditionally" aged on oak.

Anecdotally, these processes both smooth plain spirit and speed the aging process on oak. We're interested in quantifying how exactly.

That said, there might be a different format (design of experiments?) or set of variables you are interested in exploring.

Finally, in case you want some background, the initial forum where these ideas were presented is here: http://forum.moderndistiller.com/viewto" onclick="window.open(this.href);return false;" rel="nofollow ... =34&t=1883

It then jumped to this, more established, forum: viewtopic.php?f=4&t=38991

Like most forum threads, they are full of meandering conversations and deadends, but I think you'll get the general sense of the conversation in the first few pages.

Thanks again. I look forward to talking with you soon.

BADGER

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Hi BADGER,

Took a look through the forums. My first thoughts:
I like your sample schema. Our GC is set up to look for congeners primarily but we may pick up some ethyl esters as well, just haven't had enough time to look. Kara is looking into that over the coming weeks for a project we're working on anyway so we'll have some info on that shortly. I think it would be worth examining whether the effects are more pronounced at higher proofs. I thought I saw that someone had tried it at 80 but most were using barreling strength so let's make sure at least some of the samples are not diluted.

I would say the things we'll look for are reduction in congener concentration (I think that's was Terressentia was trying to show in their vodka) and corresponding increases in any ethyl esters we can pick up. We only need 50ml or so (2-5ml for gc, the rest to taste).

Let me know your timeline. We will probably have time to run some of these in June.
Thanks,
XXXXX

[Badger]

So on to figuring out what to test:


Ideally, I’d like to run two separate trials:

TRIAL A: to study the “smoothing” effects of microwave and ultrasonic on white spirit. Currently, opinions seem to veer between “it just boils off heads” and “it actually speeds the chemical processes that happen during aging”. I’d like to look at which is the case and if so, exactly what is happening. My initial suggestion for samples:

1. control white spirit. Tested once and then again 6 weeks later.
2. control #2 white spirit heated to 150 in double boiler
3. microwaved white spirit (minor dose TBD) using the FS method
4. microwaved white spirit (major dose TBD)
5. ultrasounded white spirit (minor dose TBD 40Khz?)
6. ultrasounded white spirit (major dose TBD 20 Khz?)

Questions for HD:
- other variables that are worth looking at? Suggest away!
- the distiller wants to look at alcohol %. Should EACH sample be duplicated at, say 60% and 85%? Or just, say, samples #4 and 6?
- stability seems to be an issue for some people. Should some/all of these samples be tested again after a certain time period?
- is the ultrasound power a variable?
- who out there (ideally stateside) has a ultrasonic cleaner? I’d rather not buy one just for this trial, if I can avoid it.

TRIAL B: to study the “speed aging” effects of microwave and ultrasonic on white spirit and oak. Currently, the almost-consensus seems to be that the heat and vacuum simply “sucks” flavors from the oak. I’d like to see if a). the same flavors are extracted as with traditional aging, b). whether the heating of the wood (at least with microwave) somehow changes the flavors that are extracted.

1. control white spirit
2. control #2 white spirit traditionally aged on oak.
3. control #3 white spirit “speed aged” with vacuum (no or minimal heat)
4. white spirit microwaved with oak (FS Method)
5. white spirit ultrasonically aged with oak.


Questions for HD:
- should there be a JD chips vs. oak stave trial?


So there it is. I look forward to hearing all your suggestions and thoughts.

Badger

[Badger]

I hope that Odin and Bushman will chip in with their ultrasonic experience. It is looking like I might just have to buy my own cleaner...

Some questions for them:
1. Odin - in reading your past thoughts, it seems that you feel the ultrasonic accomplishes the first 4-5 weeks of aging. Would this trial be more effective (in the sense of seeing profound effects) with brand new spirit? I currently have a stock pile of white whiskey I was planning to use but it has been aging for about 2 months. Would that make the ultrasonic effect negligible? I can make more or possibly get the distiller to contribute some of his own, if you think that's helpful.

2. If I end up buying my own, is it worth getting a beefy version like this: http://www.ebay.com/itm/TOP-SET-INDUSTR ... 45fcce21a0" onclick="window.open(this.href);return false;" rel="nofollow
What features do you find best?

3. This model can switch between 40KHz (which is evidently gentler) and 20KHz (which is rougher). Do you have a recommendation for which level to use with spirits? Should that be one of the variables that we study? Is it worth finding a cleaner that can handle a range, rather than just the two settings?

Thanks in advance,
Badger

[bellybuster]

following with great interest.

I think for any quantifiable results the samples must be identical spirits all from the same bottle/batch all of the same proof/blending. Any changes in samples will result in more variables that can be blamed for differences found..if any.

Good on you and your new acquaintances for taking this on, very interesting indeed. I wish I were able to help.

[Odin]

The newer the product, the more impact US cleaning has, yes.

I have a 2 liter 50 watts, 20 k/40 khz that works great. use the 40 khz at max. wattage.

Odin.

[Badger]

@Bellybuster- I agree absolutely. I have 3 gallons of super-basic 2-row white whiskey that I was stockpiling to do some aging experiments. I'll blend it and take all samples (including controls) from that stock...unless the distiller is willing to comp me all the booze for this! He has a freakin' humungous continuous still...he wouldn't even miss it!

@Odin - I was afraid of that. Now I have to figure out how to distill enough stock in a week or so for this whole project! Certainly, then we'll look at an ultrasounded vs. control immediately and then the same samples again after, say, 6 weeks to see if the control "caught up" or if there are still some permanent differences. So you don't use the 20 Khz, even though it seems to be more "violent"? Also, does there seem to be a minimum batch size for ultrasounding or could you use a very small amound (2-300ml).

Thanks all, for your thoughts.

Badger

[frozenthunderbolt]

Watching with great interest here: would love to justify buying an US unit; they're just so damn pricy here in nz

[Bushman]

The newer the product, the more impact US cleaning has, yes.

I have a 2 liter 50 watts, 20 k/40 khz that works great. use the 40 khz at max. wattage.

Odin.

+1, I have the same machine just a bit smaller as mine holds 1/2 gallon. So far I've been very happy with the results.

As for testing with the same run, if you are testing large quantities I am not sure this is as important as collecting multiple runs just make sure you blend them all together in the same container before dividing for testing so your samples are the same.

[Badger]

Good point. I had been stockpiling runs of white whiskey to do just that. Now, it seems ideal to do the trials on fresh distillate so I'll have to make a new series of batches and distill them all within a few days of the testing. I don't mind the actual stilling but it will really tax my meager collection of fermenters. . I think I'm going to need about 4 liters of 60% for the trials. Should be fun.

Ideally, we'll start with white spirit first and just concentrate on the polishing/aging aspects.

I'm thinking:
1. control untreated (tested immediately and at 6 weeks)
2. Control#2 heated to 150 in double boiler
3. Control #3 heated to 150 3x in microwave
4. Sample ultrasonic-ed 3x @ 40khz
5. Sample ultrasonic-ed 3x @ 20khz
6.Sample ultrasonic-ed 9x @ 40khz
7. Sample ultrasonic-ed 3x @ 40khz. (85%)

Hopefully, this will shed light on
1. Effects of microwave vs ultrasound vs heat
2. Whether ultrasonic cleaning faithfully accelerates the aging process
3. Ideal ultrasonic settings


Anyone have suggestions for other samples that would shed light on something interesting? (Oak aging will come later)

[Bushman]

Not scientific but did several tests yesterday.

Had some homemade Grand Marnier that I made 2 months ago and the only difference tasting it side by side with the commercial was the commercial was 40 proof and mine as close as I could calculate was around 67 proof. When giving it 3 treatments noticed a slight smoothing but wouldn't have had I not been looking for a change. This I think was due to the fact that it had already had time for infusion.

Later I had just made cuts from a SF/UJ combination run and put 1/2 on oak chips and did 3 passes with the ultra sonic treatment with the JD chips added. Big difference in color and taste between the 2. My conclusion is that over time aging will equal them out and improve flavor, by no means does it replace aging but as Odin said it probably gave it a boost/head start.

[Odin]

Exactly my feeling, Bushman!

Odin.

[BoomTown]

I'm thinking:
1. control untreated (tested immediately and at 6 weeks)
2. Control#2 heated to 150 in double boiler

Badger, That double boiler stuff is intriguing. BTW, how long did you hold Control#2 at temperature? When you finished this cycle, did you do any tastings? If so, what were your impressions?

Inquiring minds want to know!

[Badger]

@Odin/Bushman - interesting. I hope to be able to validate your hypothesis. If it's true, I wonder how Terresentia's process differs and/or whether it's basically a sham.

@Boomtown - to be clear, I have not done these trials yet. I hope to in about 2 weeks. I am posting these ideas now to solicit ideas for further refinement of the process. As soon as I have results, I'll post them here. The double boiler method is something I've heard of others doing...I'm mainly including it to have a treatment that is "heat only" to compare to the microwave treatment of the same temp.

Thanks all,
Badger

[Odin]

Difference is (I think), they also add oxygen to the likker. I do it too. Only not pure oxygen, but just air with a fish tank bubbler.

Odin.

[Bushman]

Difference is (I think), they also add oxygen to the likker. I do it too. Only not pure oxygen, but just air with a fish tank bubbler.

Odin.

Interesting, seems like I'm following you around Odin, can you give me a heads-up on the next new trials you are doing?

[MDH]

Difference is (I think), they also add oxygen to the likker. I do it too. Only not pure oxygen, but just air with a fish tank bubbler.

Odin.

That's safe to do with alcohol?

[Badger]

Looks like this is a topic the pros are also discussing:

http://adiforums.com/index.php?showtopi ... entry20052" onclick="window.open(this.href);return false;" rel="nofollow

[MDH]

My breath is bated.

Have there been any updates on this?

I would very much like to know if this actually accelerates chemical reactions in plain white spirits.

[Badger]

Alas, there have been some communication problems with the pro distiller.

I didn't want to distill and treat until we had a hard date set for sample delivery (since it seems that time may be a major factor with this method. I haven't heard back yet and left today for 2 weeks of vacation.

It will now be the beginning of July before I can deliver the samples.

So I still can't speak to the chemical properties but can say the ultrasonic is pretty awesome for macerations. Haven't a done a side-by-side with the nuking process, though.

As soon as I hear anything, I'll update

Cheers,
Badger

[FullySilenced]

well i can say the fruit nukin's are really really awesome as well....

[nabtastic]

i'm not much of a chemist but was wondering... the common idea is that US force oxidizes the spirit and MW boils it off (via heating and agitating the molecules). Could it be that US and MW agitate and release the oxygen trapped in the liquid from proofing water, falling from parrot, etc? I don't know if there is any merit to this, but thought we may address the issue from the other side.
NAB

[Badger]

That's a good question. One of the samples we plan to look at will be uncut, US-ed 92%. That should show us if there is a reaction (or more or less of one) with the spirit compared with the watered down 60%.

I'm meeting with the lab tech next week to work out details. Hopefully, I'll have more info soon after that.

Badger

[nabtastic]

did we ever get an update on this?

[Badger]

Samples are at the lab. Unfortunately, the lab tech went on vacation soon after i dropped them off so while I believe she ran the samples, she won't get the results back to me for another two weeks or so. This is ok because it gives me a chance to make some nuclear speed aged whiskey with the same control distillate. She'll be able to look at the effects of ultrasonically cleaning (and maybe vs microwave finishing) that when she returns. Unfortunately, I won't be able to have her test the chemical differences between speed aging and traditional aging this time around. I know we'd all like to see the results of that.

I'll post the results as soon as I get them.

Cheers,
Badger

[Bushman]

Thanks Badger for taking this on, I know a lot of members are interested in the results. Me for other reasons than aging!

[Odin]

Please keep us posted, Badger!

Busman, I have been way to busy with other things to do much more research on this topic. I guess I will await Badger's outcomes!

Odin.

[Badger]

I'm looking forward to seeing the results as much as anyone. Of course, no matter what they are, people will debate the methods or will want further testing. It's a first step anyway.

I'm hoping that I'll be able to do further work with these folks but I suspect that right now, I'm just lucky that our interests just happen to be aligned at the right time. If this trial shows nothing significant, they'll likely move on. If it shows promise, they'll probably just take over the trials and work with their own product (that's what I would do anyway). Either way, I suspect that I won't be able to leverage this partnership for very long after this initial set of samples. Hopefully, at least, if they do continue to do tests, they will share their data with me (I offered to loan them my US cleaner) and thus, with you all. Ideally, I'd love to continue working with them looking at speed aging techniques as that is a bit of a holy grail for both the hobbyist and craft distiller. We'll see...

Bushman, when things settle a bit for me I'd like to pick your brain regarding using the US for macerations. The little I've done so far has showed real promise...

Cheers,
Badger

[nabtastic]

I've heard *read- never tried myself* that US works with wood chips as does microwaving.. I'm not sure why it wouldn't work with herbs n berries - if it ever did at all. I'm particularly interested in what happens to the oxygen in the liquid as this *could* help with brewing as well, provided you had a sealed container like a keg...

At any rate, I didn't mean to pressure I you just wanted to make sure I wasn't missing anything! I'm also hoping that this will work out and we can implement this tek in the distillery ... which in turn would be a positive nod to the home distiller leading innovation in the commercial market (should help the legalization issue). oh the possibilities...

[nabtastic]

uh, badger?? you in there? still alive buddy?! haha probably got ahold of some rip vanwinkle stuff..

[Badger]

Still here. Been super busy with the school year starting and doing my first Ironman last weekend.

The samples are run but the lab tech seems to be dragging her feet to give me the numbers. I'll shoot her another email to ask for them. I suspect the results were inconclusive or else they would have been clamoring for follow up tests.