Ultrasonic Lab Trials

Treatment and handling of your distillate.

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Bushman
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Re: Ultrasonic Lab Trials

Post by Bushman »

I have not done anything with the actual fermentation but have experimented a lot with infusion of different flavors and using wood sticks and chips for flavor enhancement with positive results.
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Re: Ultrasonic Lab Trials

Post by francis »

I think I will experiment with an cheap ultrasonic fog maker.

Something like this 12v transducer on ebay:

http://www.ebay.com/itm/Ultrasonic-Mist ... 58b2fec40a" onclick="window.open(this.href);return false;" rel="nofollow
Last edited by francis on Sat Jun 13, 2015 1:55 am, edited 1 time in total.
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Re: Ultrasonic Lab Trials

Post by francis »

RandyMarshCT wrote:francis, this is VERY interesting! The 20% duty cycle seems to be the threshold.
The pictures and graphs indicate that, but they don't say what the time period of the full cycle is, unless I missed it.
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humbledore
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Re: Ultrasonic Lab Trials

Post by humbledore »

How is polyethylene alcohol safe?
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Re: Ultrasonic Lab Trials

Post by francis »

HDPE chemical resistance charts: https://www.thermoscientific.com/conten ... 20480~.pdf" onclick="window.open(this.href);return false;" rel="nofollow
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Re: Ultrasonic Lab Trials

Post by Odin »

I rather see you buy something out of SS all the way. Like this:

http://www.ultrasoonreiniger.com/emag-emmi-30hc.htm" onclick="window.open(this.href);return false;" rel="nofollow

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Re: Ultrasonic Lab Trials

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Odin wrote:I rather see you buy something out of SS all the way. Like this:

http://www.ultrasoonreiniger.com/emag-emmi-30hc.htm" onclick="window.open(this.href);return false;" rel="nofollow

Regards, Odin.
You can buy them a lot cheaper on ebay below is a 1/2 gallon + (2L) similar to mine for $82.00, you can also get a 6L for $100.00 more.
http://www.ebay.com/itm/Stainless-Steel ... 0637021944" onclick="window.open(this.href);return false;" rel="nofollow
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Re: Ultrasonic Lab Trials

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Bushman wrote:
Odin wrote:I rather see you buy something out of SS all the way. Like this:

http://www.ultrasoonreiniger.com/emag-emmi-30hc.htm" onclick="window.open(this.href);return false;" rel="nofollow

Regards, Odin.
You can buy them a lot cheaper on ebay below is a 1/2 gallon + (2L) similar to mine for $82.00, you can also get a 6L for $100.00 more.
http://www.ebay.com/itm/Stainless-Steel ... 0637021944" onclick="window.open(this.href);return false;" rel="nofollow

Nice. Thanks for the link. Ok you guys convinced me the ultrasonic fogger would not really work (not 20W per liter). I'll get a 2L ultrasonic cleaner. How long do you treat it for? I notice most of these units have a 30 min timer.
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Re: Ultrasonic Lab Trials

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I give it 3 10 minute baths with a 15-20 min rest in between.
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Re: Ultrasonic Lab Trials

Post by Odin »

Same procedure here. Adding oxygen even helps improve results.

Odin.
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Re: Ultrasonic Lab Trials

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Odin wrote:Same procedure here. Adding oxygen even helps improve results.

Odin.

Has anyone here tried adding a bit of hydrogen peroxide to accelerate aging ?
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Re: Ultrasonic Lab Trials

Post by kiwi Bruce »

It's a brave new world boys and girls. I think we are seeing a new window of opportunity opening before our eyes. A new class of Beijing capitalists is emerging, with a desire for western cigarettes and a thirst Western spirits, and it's a market that is only going to get bigger. Commercially available, fast maturation for the spirits industry is the obvious answer. It's exciting to see everyone's input and the progression of ideas. I hope some of you think of taking this into the commercial arena, after all, there is a dragon to feed! Kiwi Bruce
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Re: Ultrasonic Lab Trials

Post by francis »

I've used an airstone on a liter of heads that had a strong smell, of what I assumed was acetone. But it was very probably ethyl acetate. After bubbling for a day in a cool garage volume down by 5% and acetone smell greatly reduced, but still detectable. I may try ozone, as I have an ozone bubbler. This came off a turbo wash, before I knew any better.
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Re: Ultrasonic Lab Trials

Post by Bagasso »

francis wrote:I've used an airstone on a liter of heads that had a strong smell, of what I assumed was acetone. But it was very probably ethyl acetate. After bubbling for a day in a cool garage volume down by 5% and acetone smell greatly reduced, but still detectable.
5% seems like a lot. It might be that introducing air into the distillate was causing the production of ethyl acetate at the same time that it was airing some of it out. A possible solution would be to raise the pH to counter the production of ethyl acetate but the drawback would be that you would loose some/many of the esters wanted in a flavored distillate, if that is what you are after.
I may try ozone, as I have an ozone bubbler.
This is something that I have wanted to try but don't have the generator. The same problem/solution above would come into play.
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Re: Ultrasonic Lab Trials

Post by francis »

Bagasso wrote: 5% seems like a lot. It might be that introducing air into the distillate was causing the production of ethyl acetate at the same time that it was airing some of it out. A possible solution would be to raise the pH to counter the production of ethyl acetate but the drawback would be that you would loose some/many of the esters wanted in a flavored distillate, if that is what you are after.

This is something that I have wanted to try but don't have the generator. The same problem/solution above would come into play.
Yes, it's introducing a ton of air into the distillate :-) I did try sodium bicarbonate, after my stripping run, not on the jar of the second pass distillate, which was 80%.

Ozone bubblers are < $20 on ebay or ali express. I use one for treating sprouts when they are done:

http://www.ebay.com/itm/200mg-hr-Fruits ... 3cea903948" onclick="window.open(this.href);return false;" rel="nofollow

http://www.aliexpress.com/item/Free-Shi ... 30415.html" onclick="window.open(this.href);return false;" rel="nofollow
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Re: Ultrasonic Lab Trials

Post by Bagasso »

francis wrote:Yes, it's introducing a ton of air into the distillate :-) I did try sodium bicarbonate, after my stripping run, not on the jar of the second pass distillate, which was 80%.
Any bicarb used in low wines wouldn't come over on the spirit run.
Ozone bubblers are < $20 on ebay or ali express.
Thanks, I have seen them but since I don't really have any other use for one I am on the lookout for positive results before deciding.
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Re: Ultrasonic Lab Trials

Post by francis »

Well I'll be dammed . . . it really works ! :-)

I did order a 2L SS unit, but in the meantime I looked for my ultrasonic fogger. But could not find it.

But I did find an ultrasonic mister / humidifier, that you screw on to a water bottle and plugs into a USB port. It outputs 2W.

Image

I just set the cap on the ground and set a mason jar of some fresh distillate with some fruit from a can on it.

I had two jars, filled each to the same level (1/3) with lychees and syrup from a can, and the rest the fresh distillate. Same volume for both jars.

So one jar on the mister and one off. Since it's only 2W, I let it run for 24 hours.

I can smell low concentrations of ethyl acetate (acetone smell) easily.

The jar on the mister is noticeably clearer (interesting because you would expect vibration to maintain turbidity).

The acetone smell is very faint. It's very smooth, sweet tasting.

The jar off the mister is more cloudy and still has sharp acetone smell.

Temperature is the same, ambient 20C. The difference in smell is very noticeable after 24 hours.

Now trying hydrogen peroxide (1/4 tsp of 3% hydrogen peroxide in the quart mason jar of alcohol) plus the cap mister . . .
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Re: Ultrasonic Lab Trials

Post by francis »

You can make an ultrasound treatment device for about half the price of the ones on ebay.

I don't need the heater. I want to treat the distillate at room temperature or below for a longer time.

So I just need a driver board and a transducer. Epoxy the transducer to the bottom of a thin stainless steel mixing bowl from the dollar store and off you go.

100W 40kHz power driver: http://www.ebay.com/itm/100W-40KHz-Ultr ... 2800eb9d89" onclick="window.open(this.href);return false;" rel="nofollow

60W 40kHz transducer: http://www.ebay.com/itm/1-60W-40KHz-Ult ... 3aaa187e00" onclick="window.open(this.href);return false;" rel="nofollow
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Re: Ultrasonic Lab Trials

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https://www.youtube.com/watch?v=1EH6atYydBc" onclick="window.open(this.href);return false;" rel="nofollow
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Re: Ultrasonic Lab Trials

Post by johnnyv »

Am I missing something?

From the results the microwaved material appears to be superior.
Removal of all ethyl acetate without concentrating the higher alcohols, presumably by not evaporating as much ethanol.

https://en.wikipedia.org/wiki/Microwave_chemistry" onclick="window.open(this.href);return false;" rel="nofollow
Sometimes use this at work, can get reactions to occur at fairly low temperatures compared to conventional heating.
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Re: Ultrasonic Lab Trials

Post by Bagasso »

johnnyv wrote:Sometimes use this at work, can get reactions to occur at fairly low temperatures compared to conventional heating.
I found this: MICROWAVE CHEMISTRY — AN APPROACH TO THE ASSESSMENT OF CHEMICAL REACTION HAZARDS

Seems like things shift quite a bit in a MW. On page 6 there is an interesting table that shows that under something they call microwave conditions things have the following boiling points:

Solvent			°C

Water 			104
Dimethylformamide 	170
Acetonitrile 		107
Methanol 		84
Ethanol 		103
Acetone			81
Dichloromethane 	55
Tetrahydrofuran 	81
Ethyl acetate 		95
Propan-2-ol 		100
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Re: Ultrasonic Lab Trials

Post by johnnyv »

That is a good paper!

Household microwaves are at a frequency that penetrates water, less efficient but used so food is heated more evenly rather than just heating on the outside.
It is possible that some of these polar solvents are absorbing the energy more easily and getting preferentially heated.
Also water has a very high specific heat compared to most solvents, usually around twice the energy required to raise its temperature.
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Re: Ultrasonic Lab Trials

Post by Bagasso »

johnnyv wrote:It is possible that some of these polar solvents are absorbing the energy more easily and getting preferentially heated.

Also water has a very high specific heat compared to most solvents, usually around twice the energy required to raise its temperature.
I had just given it a quick glance and that table jumped out at me. Looking at the paper slowly I see that it has very limited application to distilling. Seems like they are focusing on single solvents in a microwave.

Still the most significant bit is the shift in boiling point for ethanol from 79°C to 103°C. While methanol, acetone and ethyl acetate shift to 84°C, 81°C and 95°C respectively. Even propan-2-ol sneaks in under ethanol at 100°C. So in theory you should be able to drive off these 4 congeners (maybe even others that just were not on that list) a lot easier due to the shifts in BPs.

The one thing that is of concern, and it is the reason the table of BPs is in there, is superheating.

Say you take a liter of low wines and heat in a MW to 102°C. In theory you will have gotten rid of a fair amount of the congeners mentioned above but as soon as you disturb or add something to the liquid both the water and the ethanol are going to want to boil off instantly.

I took 125ml of wine and heated up to around 92°C and when I dropped my thermometer probe in I got a bit of a surge from the wine. Nothing dangerous (probably because it wasn't to far over the bp of etho and still below water) but it was still a reminder of what to take into consideration.

Might look further into it and start a thread instead of further derailing this one.
Last edited by Bagasso on Wed Apr 12, 2017 5:30 pm, edited 1 time in total.
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Re: Ultrasonic Lab Trials

Post by droo1966 »

As a member who distress ages azeotrope using hot water as opposed to the microwave method, I'm following this thread very keenly.


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