Ultrasonic Lab Trials

[nabtastic]

Ironman? heavy bro. congrats on even attempting that!

[Badger]

It was a lot of fun. A mch ucheaper mid-life crisis than buying a Corvette.

Here's the lab tech's latest reply:
"I'm so sorry about the delay in this, I have been so incredibly busy lately! I am going to be working on getting all of the data together to see if there is any other differences, but initially all of the samples were very close on the fusel alcohols, so I'm going to be looking to see if I can find any other variations. Tasting them there is a bit of difference, but again I just need to find the time to calculate some more results. I will have some more time at the end of this week, so I will definitely be sending you more then."

That was sent on the 3rd. I'm trying not to hound them too much as I don't want to scuttle a possible cool relationship. Still, like I said before, I think they'd be making more of an effort if they saw some really amazing results. The samples I gave them were all white spirit... the only aged I could give them was speed aged with the nuclear method and I screwed it up. Now, they don't seem interested in getting higher quality aged samples. I've offered twice and they've effectively ignored that part of my emails. Sooooooo, I'm guessing this will probably be it. I'll shoot her another email this week... we'll see what I get.

[nabtastic]

In this case, a lack of definitive results is not necessarily the worst thing ever. Even something that is not chemically all that different can be perceived as tasting/smelling considerably different. To my knowledge I have never tried this company's products but Terressentia offers these results: http://www.terressentia.com/terrepure/research

In my experience, aging in a plastic (read: gas permeable) container actually reduces the harshness considerably in the first few weeks. This, of course, doesn't make a bad spirit good - only better. After the first few weeks I haven't been able to notice much of a difference. I will be building a US test chamber to experiment with products and sending them to a TTB approved lab. It'll take me a few months to get it all together I'm certain, but i'll post an update if I ever get it finished.

[MDH]

Amyl alcohol content is not important. The going hypothesis is that ultrasonic energy combined with aeration creates a form of cavitation that evaporates light compounds. Terressentia recommends to pair it with aeration. From my limited understanding of this - so take it with a grain of salt - essentially you are just performing aeration but the ultrasonic technology affects how the aeration occurs inside the spirit, resulting in smaller bubbles, and thus performing a form of aeration that is less crude/rough and more thorough.

What I'm interested in is if it actually affects esterification. There are studies done on wine that suggest microwave energy speeds ester formation. Does ultrasonic?

[Max_Vino]

Hi Badger,

What I would be interested in seeing is how a blind tasting compares with the lab results. I think it would be important to have 3-4 tasters. Hopfully there would be some agreement on which samples were performing best.

Cheers,
Max

[nabtastic]

MDH, forgive my ignorance, but what do you mean when you refer to esterification?

Thanks,
NAB

[Badger]

Ethyl Acetate.pdf

(176.37 KiB) Downloaded 498 times

Ok. So after a looooong time, I finally got the results back from the lab. In my opinion, they are fairly underwhelming in the sense that there is not some obvious amazing result. Still, some of you may be able to do more with the data than I. I'm including the lab tech's final email along with the data. Just in case the formatting gets screwed up, I'll also attach a pdf of the excel doc they sent me. I tried pasting the data but can't seem to get the formatting right.

A few notes about the testing:
1. All samples came from a common batch of white spirit and were about 200ml.
2. Sample size was a major flaw in the testing as it was small enough that the US vibration would heat it up (even when I turned the heat OFF). That HAD to create some inconstancy, and considering how minor the results were, I'm guessing renders much of the data fairly moot. If I were to do this again, I'd use at least a liter per sample.
3. The "indirect heat" was done with a double boiler method. O2 was added with an aeration stone.
4. They did not, to my knowledge, retest the control after 6-8 weeks to see if the US just accelerated the natural aging process. I'm bummed about that as I was very interested in that.


"So the initial results I got on our GC showed a slight reduction (by ~a factor of 10) in the ethyl acetate for all methods compared to the controls, but since that is very volatile even slight amount of heat can cause a drop in that. Everything else seem to stay relatively close to where the controls were. The other congeners we have quantified so far are n-propanol, isobutanol, n-butanol, amyl alcohol, and methanol, which you will see the results attached with everything there except the methanol, which none of your samples had enough to register. I also had ran the samples with the oak extract in them, but I didn't include the results mainly because the congeners we had identified can't tell us much about the extracted oak."

Ethyl Acetate.pdf

(176.37 KiB) Downloaded 498 times

Ethyl Acetate / n-propanol / isobutanol / n-butano l / amyl alcohol
87% Control 0.11816 / 0.51485 / 0.64813 / 0.00245 / 2.098
87% 20 min at 40kHz 0.069 / 0.52906 / 0.67883 / 0.00267 / 2.209
87% 20 min at 20kHz 0.032716 / 0.5721 / 0.7171 / 0.00381 / 2.777
87% 20 min at 40kHz with O2 and heat 0.01807 / 0.580488 / 0.7256 / 0.00413 / 2.955

60% Control 0.031295 / 0.27023 / 0.40784 / 0.001445 / 1.639
60% microwaved to ~170 0 / 0.2312 / 0.36405 / 0.001264 / 1.5698
60% indirectly heated to ~170 0 / 0.35225 / 0.38867 / 0.002104 / 2.033
60% 20min @ 40kHz 0 / 0.26371 / 0.38572 / 0.001746 / 1.8237
60% 20min @ 20kHz 0 / 0.26347 / 0.33816 / 0.001342 / 1.6974
60% 20 min @ 40kHz with O2 and heat 0 / 0.23331 / 0.36802 / 0.00137 / 1.6389

[aj2456]

just found this cool little thread, shame they were a bit busy/ lazy intern (or should i just say standard intern), and gotta commend you on taking the initative and looking into this professionally-
Anyway regardless you must be well pleased they couldn't even detect any methanol in the samples

oh well guess its back to the good and cheap biological spectometer aka tongue

[Odin]

Badger,

Go buy glasses right now! And congrats! Your findings, though dissapointing to you, are NOT disappointing to me. USC treatment helps lower the amount of ethyl acetate by a factor 2 to 3.

And that it does not have an effect on most of the alcs present ... that's not surprizing. At least to me. I have always said it USC helps you get rid of ethyl acetate. And the numbers show just that.

I disagree with the researcher that the outcomes are corrupted because the samples were so small they heated up.

Off course they heat up! Bigger samples will heat up just as fast, given the fact that you should always do USC in such a way that there is a minimum wattage of power input per liter (20 watts per liter actually). And it is the actual USC treatment that puts the power in. Without that no heating up, but without that no USC either.

The great outcomes for USC cannot be described to heating. Why? Look at the indirectly heated portions that have been tested.
Congrats to all of us investigating this: USC greatly reduces the amount of ethyl acetate, especially when oxygen is introduced.

What I have been telling from the start. Great to see it proven by lab results. Thanks for the effort you put into it Badger. Very much appreciated.

The other factions are not so much affected. Makes sense. It is the ethyl acetate that binds with oxygen we were after here. To reduce the amount of "vinigar accid", because that's what ethyl acetate is. That reduction hugely improves the drink. Just imagine putting just one drop of vinegar in your bottle of wine and you understand the huge impact ethyl acetate and USC can have.

I think we have a taste receptory of around 1 to 2 ppm on that darn ethyl acetate. Imagine USC helps us bringing it down from - say - 2 to 1. Makes all the difference!



Odin.

[Badger]

Odin -

Way to make me feel good. As an English major, all these number-y things just befuddle me. If you need a metaphor for your booze, I'm your man. That said, your comments help me understand why, even though the numbers all look very similar to me, the tech did mention that they noticed a discernible difference when tasting my samples.

I was really hoping to have them run some oaked samples (I offered some multiple times) and they had initially indicated a lot of interest in doing that. That said, I had to get so pushy just to get these #s, I don't think that will happen very soon. I don't want to rip on them...aj2456 was right about the intern, sounds like she is crazy busy with much more pressing stuff than our little side research. Still, I'm bummed we can't explore more, at least for now.

My bottom line: it sure looks like US doesn't hurt and I now have the damned machine, I might as well use it. I'll treat most of my product. It certainly rocks for macerations...I make a cinnamon vodka in 30 min that used to take me a month of steeping.

Cheers to all,
Badger

[Odin]

No!

No, Badger. Bottom line is: USC helps you clean up your product and brings ethyl acetate levels to or within acceptable levels in no time. That's an increadible achievement in a short period of time. Glad I found the reviews from 1930's and 1950', and re-introduced it on this forum (and with most of my micro distillery clients actually, and with great success).

And just to give you an idea: blind tests in the 1950's showed that, on a 10 point scale, a whiskey judged with a "7" would get an "8" after USC treatments. And a 3 year old would be mistaken for a 5 or 7 year old whiskey.

And I agree with the researcher: oak has no meaning here. Not in these tests.

Only thing you are doing by micronizing or USC-ning with wood is ... you are measuring extraction. Interesting, from a science point a view, but not from a chemical point of view. Yes it extracted faster. Or not. May have been the heat, may have been the wood.

None of the chemical compounds in the likker are "hit" as hard as ethyl acetate. No chemistry major. Not even a minor (I think), but my explanation is: ethyl acetate reacts with oxygen to form X and Y (forgot what Y is, but me thinks X is actually ethyl alcohol). Oxygen gives less ethyl acetate = less vinegar = less of that sharp bite associated with young drinks.

Ultrasonic works as follows: the intense vibrations causes micro bubbles/pockets of air creation that instantly blow up (due to the same high frequency vibrations). The creation and collaps causes two things:
1. Ethyl acetate / oxygen contact during the air pocket creation phase, minimizing actual ethyl acetate numbers in the drink;
2. Molecules meeting during the collapse phase: faster esterification.

Now the esters weren't into the equasion of your research, I think, even though, on the 40 khz USC trials, I saw some increase in most other alcs. May be due to evaporation of the other elements or be part of that exact ageing process that's speeded up USC wize.

My point? This is no small achievement. USC really helps you to make a more drinkable product sooner (e.g. see the 3 vs 5/7 years old whiskey example). And it helps pro distillers to bring a better product to the market sooner. Especially suited for vodka's, but also for brandies and American whiskey.

Not so much for Scottish whisky, since over there it is the age stamp that defines the value, not the quality of the drink. Rephrase: it is the age stamp on the bottle that defines perceived quality of drink by their consumers. That and the ever increasing price tag!



Odin.

[Badger]

Odin -

Thanks for the great comments; you've given me a lot to think about. I'm curious though, what is your "no!" in reference to? I'm not clear on which of my statements you are disagreeing with.

And to be clear, the oaked samples I was hoping they would test were not USC'ed WITH oak, just treated AFTER being on oak (specifically, I used the nuclear aging process). Since part of the question of US revolved around the idea of "speed aging", I was hoping they would be able to quantify that 3 year--> 5 year whiskey dynamic. Oh well, maybe next time.

And I did ask them about esterification but she never responded to that specific issue: either their test did not address it, they wanted to keep the results to themselves, or she just didn't get around to it. Bummer, no matter what.

cheers,
Badger

[Bushman]

Just remember I was second behind Odin in this discovery and use....dang I'm tired of being a day late and a dollar short!

[Odin]

For me the situation is slightly different. One day quicker but a grand short!



Odin.

[nabtastic]

Excellent results. I was hoping this would hold true. I'm working on a bulk spirits fill method using a keg and compressed oxygen. will probably fix some US equipment to it. Any thoughts?

[Odin]

Don't forget the Ultra Sonic part!

Odin.

[nabtastic]

I was thinking something like this http://www.bjultrasonic.com/135khz-50w- ... Ogod1RgAoQ
I read a "how to" the other day using much more expensive pieces, but figure this should work since it's a non-critical part.

[Odin]

Not sure. Very high frequency. 20 and 40 khz are tested and good. On 135 khz ... no experience there. And select one that has at least 20 watts per liter it can contain.

Regards, Odin.

[nabtastic]

well, guess it's time to do some experimenting. thanks Odin.

NAB

[Badger]

Odin - a quick follow-up question:

I'm not familiar with the chemistry of aging but is the conversion of ethyl acetate something that would happen naturally, say in a barrel? Is this what we discussed earlier as something that natural aging would "catch up" with in 3-6 months? If so, is it fair to say that this would be a process that would benefit vodka or other immediately bottled spirits but would be essential for something like whiskey, which will age for quite a while?

I really wish the lab had run the control again after 8 weeks, like I suggested.

Thanks,
Badger

[Odin]

Ethyl acetate converts naturally, over time, and under O2 contact.

Odin.

[Badger]

So if that's the case, then it's pretty important to find out if USC affects esterification at similar rates. If not, then there's not much point to treating something that will still have to be aged for a traditional amount of time (for esterification and oak flavoring).

Would it be fair to say that this process is currently best for white spirits (vodka, white dog)? What about gin? I'd think the strong juniper flavoring would mask any minor ethyl acetate off flavors?


thanks,
Badger

[Odin]

I think it is good for any drink ... if you feel you want to speed up the process. Gains on white drinks are limited to 5 weeks (normal ageing time for white). But gains on whiskey are much bigger, timewise.

Odin.

[Badger]

Hmmm. So let's see if I get this straight :

In traditional barrel aging, there's flavoring (with oak flavors begin leached from the wood) and then the chemical aging process. This chemical process involves a). the chemicals in the distillate interacting with the the chemicals in the oak extract (which I'm imprecisely calling esterification) and b). the chemicals in both interacting with oxygen.

The ethyl acetate conversion is the distillate (independent of whether it has been oaked) interacting with the oxygen.
Are you claiming that US+O2 also speeds up the esterification (when it HAS been oaked)?

If so, does the esterification and oxidation take approximately the same time (traditionally) or is there value in accelerating one or the other? And is there most value in doing the treatment BEFORE the oak chemicals are introduced, during the aging process, or at the end, once the spirit has been sufficiently oaked?

man, i wish I had been a chemistry major and not an english major.

Thanks,
Badger

[Odin]

Shit, you askin' Q's here. With a capital.

Not sure I can answer.

But, here is where the true advantage of US comes into play: 2 dimensions meeting 3 dimentsions.

Talking "Startrek" to you? I haven't even started.

In a 50 to 60 gallon barrel, extraction (wood flavouring) and ageing (3 to 5 years) seem to be ... pretty much balanced out.

But start-up micro's want to bring their product to the market faster. Maybe make use of "two years on oak is enough" legal rule. But is a whiskey ready after only ageing two years? Good question.

Start-up micro's like to put their whiskey in smaller barrels. Less gallons in a smaller barrel. And that means more wood contact per gallon. So ... the wood flavour extraction part is there. With a smaller barrel you can get there sooner. But how about ageing? And there I mean: compounds meeting and taking different molecular shapes. Smaller barrels do not help a lot there.

There's two solutions a start-up micro distillery can choose:
1. Make tighter cuts. But the disadvantage is that there will be less character in the final whiskey.
2. Age for some time after the whiskey has been taken out of the barrel. But this would mean time to market is taking too long.

US treatment can get you there.

Now, towards homedistilling. Aren't our quantities (gallons) even smaller? On the other hand, we are not bothered with legal issues like "a whiskey should at least have matured for two years in a barrel", right? We can choose JD wood smoking blocks and get faster extraction. And we can use Ultrasonic Ageing to speed up the agein process.

Odin.

[Tortuga]

I know I'm a bit late on this discussion, but I noticed that on the 87% samples there was not only the decrease in Ethyl Acetate (which is a win in itself), but that there was also an increase in isobutanol (which food additive companies list as having musty or winey properties) and amyl alcohol (a group of alcohols that the food additive companies list as "sweet, vanilla").

I'm no chemist so I'm not certain if the increases are statistically significant or could be to random chance, but that looks like additional promising results for not only ultra sonic treatments but also forced oxidative treatments. There are a variety of other compounds that develop throughout the aging process (especially in rum) that would likely also be sped up by the ultra sonic and oxygen treatments.

I'm wondering if anyone else would have the ability to get some tests run. Possibly with a batch of rum and testing for various esters as well to see whether their development or degradation was affected by these processes.

I believe the science has been shown to be probable, naysayers notwithstanding. It makes sense, since there is general agreement that oxygen contact/transfer through the oak barrels contributes to the aging process. Also, it has been shown historically that barrels traveling across the ocean by ship mature more quickly than those sitting in a warehouse. Further, many distilleries know that barrels located in certain parts of the warehouse (such as near a window) that experience either higher average temps or larger temp swings will also mature more quickly. It seems to me that motion, oxygen, and some modicum of heat or heat variation all contribute substantially to the maturation process (in addition to good ingredients, of course). Why would these not be able to be forced in a more rapid manner to enhance the maturation process (really we can't call it aging with all of the variables independent of time that have been proven throughout the storied history of spirits).

If we stop using the misnomer "aging" and call it what it really is, "maturation," we can put past old prejudices and embrace new techniques for making better spirits.

[razerhawg]

Holy Frigging Smoke. I ordered a 22 litre ultrasonic cleaner. I opened it up and cleaned it out and added about 8 quarts of 80 proof to it that was kind of a birdwashers sugar wash. Heated it up to about 45c and let it run for 20 minutes....This is truly the smoothest thing I have ever drank ( it's still warm? ). I just took some heads and tails and put them in this cleaner and we will see how it comes out.

[MDH]

Why would these not be able to be forced in a more rapid manner to enhance the maturation process (really we can't call it aging with all of the variables independent of time that have been proven throughout the storied history of spirits).

They are, and in practice. Kavalan has released some truly excellent Single Malts. Their warehouse regularly reaches 35 degrees celcius. All chemical reactions proceed at a greater rate at such a temperature, and their three year olds show excellent charactaristics for such young Whisky.

[francis]

Apparently ultrasonic treatment improves the production of ethanol during fermentation.

http://www.massey.ac.nz/~ychisti/Ziad2011.pdf" onclick="window.open(this.href);return false;" rel="nofollow

This news article: http://www.ethanolproducer.com/articles ... -new-level" onclick="window.open(this.href);return false;" rel="nofollow

[RandyMarshCT]

francis, this is VERY interesting! The 20% duty cycle seems to be the threshold.