Hidden science behind normal and accelerated DIY e-Liquid steeping.

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Hidden science behind normal and accelerated e-liquid steeping.

We are all aware of the effect of steeping e-liquid can improve its flavour and change its colour.

In this article I am attempting to describe the cause and effect systems involved in e-liquid steeping and accelerated steeping from a scientific viewpoint.

There are two major processes involved in steeping e-Liquid

1. Removal of volatile components by evaporation and degasification

This process would include the removal of alcohol but is not restricted to alcohol, there are other volatile components used in the production of flavour concentrates that generally give off an astringent or chemical odour.

These process requires access to the atmosphere hence the need to remove tops from bottles

1a Evaporation – This is the same process as used in cooking to remove alcohol from wine.

1b Degasification – This is the sameprocess as letting a fizzy drink going flat

Both of these processes are accelerated by heat and increased surface area.

This is a critical first step many e-Liquids are hideous and un-vapeable before this process.

Without acceleration this can take a week or longer due to the viscosity of the liquid.

2. The development of complex flavour molecules.

Over time some e-Liquids especially custard / caramel or desert flavours darken over time

From observation this cannot be oxidation as it occurs uniformly through the liquid and does not require agitation of the liquid to occur.

It also cannot be caramelization as this does not occur below 110°C.

Maillard Reaction - Colour and flavour

What seems to be happening is a Maillard reaction commonly experienced by most people every day. The browning of bread, toast and potato chips these are high temperature examples. Medium temperature examples creating Dulce de leche and condensed milk.

Mallard reactions also occur at lower temperatures and contribute to the aging of wine and Balsamic Vinegar.

Maillard reactions get exponentially slower as they progress

This fits in with our observations of steeping e-Liquid, a golden colour may be observed in a couple of days however the full desired flavor and colour may take 4-6 weeks to develop.


The Maillard reactions will continue to progress over time, hence those almost black bottles of e-Liquid that are found at the back of a draw.

Accelerating the steeping process

Removal of volatile components by evaporation and degasification

a) Taking the top off the bottle.

Evaporation and degasification simply wont happen with the lid on (Think bottle of lemonade)

b) Shaking the bottle (Helps)

c) Stirring (Helps)

d) Whisking (Very effective)

c) Blending to a foam (Super Effective)

d) Ultrasonic degasification (Super Effective)

Video Showing Ultrasonic degasification
http://www.hielscher.com/degassing_01.htm

d) Heating to 40°C-50°C (Accelerates all of the above methods)

Maillard Reaction - Colour and flavour

a) Heating to 40°C-50°C (Maillard reactions go slower at lower temperatures)

b) Ultrasonic treatment (local extremes of temperature and pressure act as a catalyst)

In Practice

The image on the left was taken immediately after mixing the image on the right was taken 5 hours later

Steeping_zpsp3eux8si.jpg


60:40 VG PG 18% Nic 15% T-Juice Custard Concentrate

The e-Liquid was very vapeable the next day and is continuing to improve in the bottle.

Method used

a) Mixed liquid by weight directly into the blender cup.

b) Blended to a foam for 15 seconds remove lid

c) Placed into ultrasonic bath pre-heated to 50°C

d) 20 minuet ultrasonic cycle

e) 20 minuet rest

f) repeated (b) to (e) above six times

Then bottled into 50ml bottles

Storing after accelerated steeping.

Storing lid off in warm (room temp) draw or cupboard will allow any new volatiles to escape

This is less important as time passes.

The e-Liquid will continue its Maillard reaction gaining in richness, complexity and darkening
further.

There will be a point where you will not want the process to continue this is of personal preference.

This dictates how much you should make. As the Maillard reaction slows down most e-Liquids have a “Window of Niceness” lasting a couple of months.

The process can be slowed by refrigeration don’t freeze your liquid.

Quality and Issues

There is no quality related advantage accelerating the steeping of e-Liquid.

Heating some flavours may introduce unwanted cooked flavours.

If the acceleration process is overdone the “Window of Niceness” shelf life can be drastically reduced.

Full blown blending is impractical for quantities of less than about 100ml

Good old lid off in a dark place with a bit of a shake now and then will result in a perfectly steeped e-Liquid it is also far more predictable than accelerated steeping. It just takes longer.

As there are so many variables involved, you should always keep notes on how you
have steeped your e-Liquid along with the ingredients. You can then easily replicate your successes.

Joe Dyer

References

Wikipedia entry on Maillard reactions

http://en.wikipedia.org/wiki/Maillard_reaction

Description of low temperature Maillard reactions

http://cooking.stackexchange.com/questions/29926/what-temperature-does-the-maillard-reaction-occur


By

Joe Dyer
 

mikol gaither

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Jun 18, 2015
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you mentioned surface area and degassification. would you think, have you tried, a thinner layer in a wide bottom dish? Do you think the container itself can play a role in the steeping process? most of us use 15ml or whatever the case a small surface area with a LOT of liquid beneath that is restricting oxygen with the exception of shaking. just saying....
 

Tom Forde

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ECF Veteran
Mar 16, 2015
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Okay this is really interesting. I own a professional music studio, and I DIY my juice. With the untrasonic degassification, what frequencies are used? I have full range frequency spectral analysis programs on my studio's computers so I wonder if I could jerry up an old speaker's port hole to a short sterile tube to do this. It wouldn't be unreadable, as all speakers do are vibrate at different frequencies and move air to create sound, and the port hole on a subwoofer or studio monitor pushes out the reverberated air from the inside of the monitor.
 
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Sir2fyablyNutz

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I just got an ultra sonic cleaner yesterday for my DIY. (Harbor Freight $85 then a 20% coupon found online) I was amazed at how much the juices changed. This post was very interesting to understand this perspective on steeping. Thanks.



Hidden science behind normal and accelerated e-Liquid steeping.

We are all aware of the effect of steeping e-Liquid can improve its flavour and change its colour.

In this article I am attempting to describe the cause and effect systems involved in e-Liquid steeping and accelerated steeping from a scientific viewpoint.

There are two major processes involved in steeping e-Liquid

1. Removal of volatile components by evaporation and degasification

This process would include the removal of alcohol but is not restricted to alcohol, there are other volatile components used in the production of flavour concentrates that generally give off an astringent or chemical odour.

These process requires access to the atmosphere hence the need to remove tops from bottles

1a Evaporation – This is the same process as used in cooking to remove alcohol from wine.

1b Degasification – This is the sameprocess as letting a fizzy drink going flat

Both of these processes are accelerated by heat and increased surface area.

This is a critical first step many e-Liquids are hideous and un-vapeable before this process.

Without acceleration this can take a week or longer due to the viscosity of the liquid.

2. The development of complex flavour molecules.

Over time some e-Liquids especially custard / caramel or desert flavours darken over time

From observation this cannot be oxidation as it occurs uniformly through the liquid and does not require agitation of the liquid to occur.

It also cannot be caramelization as this does not occur below 110°C.

Maillard Reaction - Colour and flavour

What seems to be happening is a Maillard reaction commonly experienced by most people every day. The browning of bread, toast and potato chips these are high temperature examples. Medium temperature examples creating Dulce de leche and condensed milk.

Mallard reactions also occur at lower temperatures and contribute to the aging of wine and Balsamic Vinegar.

Maillard reactions get exponentially slower as they progress

This fits in with our observations of steeping e-Liquid, a golden colour may be observed in a couple of days however the full desired flavor and colour may take 4-6 weeks to develop.


The Maillard reactions will continue to progress over time, hence those almost black bottles of e-Liquid that are found at the back of a draw.

Accelerating the steeping process

Removal of volatile components by evaporation and degasification

a) Taking the top off the bottle.

Evaporation and degasification simply wont happen with the lid on (Think bottle of lemonade)

b) Shaking the bottle (Helps)

c) Stirring (Helps)

d) Whisking (Very effective)

c) Blending to a foam (Super Effective)

d) Ultrasonic degasification (Super Effective)

Video Showing Ultrasonic degasification
http://www.hielscher.com/degassing_01.htm

d) Heating to 40°C-50°C (Accelerates all of the above methods)

Maillard Reaction - Colour and flavour

a) Heating to 40°C-50°C (Maillard reactions go slower at lower temperatures)

b) Ultrasonic treatment (local extremes of temperature and pressure act as a catalyst)

In Practice

The image on the left was taken immediately after mixing the image on the right was taken 5 hours later

Steeping_zpsp3eux8si.jpg


60:40 VG PG 18% Nic 15% T-Juice Custard Concentrate

The e-Liquid was very vapeable the next day and is continuing to improve in the bottle.

Method used

a) Mixed liquid by weight directly into the blender cup.

b) Blended to a foam for 15 seconds remove lid

c) Placed into ultrasonic bath pre-heated to 50°C

d) 20 minuet ultrasonic cycle

e) 20 minuet rest

f) repeated (b) to (e) above six times

Then bottled into 50ml bottles

Storing after accelerated steeping.

Storing lid off in warm (room temp) draw or cupboard will allow any new volatiles to escape

This is less important as time passes.

The e-Liquid will continue its Maillard reaction gaining in richness, complexity and darkening
further.

There will be a point where you will not want the process to continue this is of personal preference.

This dictates how much you should make. As the Maillard reaction slows down most e-Liquids have a “Window of Niceness” lasting a couple of months.

The process can be slowed by refrigeration don’t freeze your liquid.

Quality and Issues

There is no quality related advantage accelerating the steeping of e-Liquid.

Heating some flavours may introduce unwanted cooked flavours.

If the acceleration process is overdone the “Window of Niceness” shelf life can be drastically reduced.

Full blown blending is impractical for quantities of less than about 100ml

Good old lid off in a dark place with a bit of a shake now and then will result in a perfectly steeped e-Liquid it is also far more predictable than accelerated steeping. It just takes longer.

As there are so many variables involved, you should always keep notes on how you
have steeped your e-Liquid along with the ingredients. You can then easily replicate your successes.


Joe Dyer

References

Wikipedia entry on Maillard reactions

http://en.wikipedia.org/wiki/Maillard_reaction

Description of low temperature Maillard reactions

http://cooking.stackexchange.com/questions/29926/what-temperature-does-the-maillard-reaction-occur


By

Joe Dyer
 
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Dom

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May 2, 2015
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Linwood, NJ
I just got an ultra sonic cleaner yesterday for my DIY. (Harbor Freight $85 then a 20% coupon found online) I was amazed at how much the juices changed. This post was very interesting to understand this perspective on steeping. Thanks.
will you pour the liquid in the cleaner or just set the bottles in there?
 
Okay this is really interesting. I own a professional music studio, and I DIY my juice. With the untrasonic degassification, what frequencies are used? I have full range frequency spectral analysis programs on my studio's computers so I wonder if I could jerry up an old speaker's port hole to a short sterile tube to do this. It wouldn't be unreadable, as all speakers do are vibrate at different frequencies and move air to create sound, and the port hole on a subwoofer or studio monitor pushes out the reverberated air from the inside of the monitor.
Very dependant on unit used about 30-40KHz even a high frequency horn could not generate the power required just get an ultrasonic cleaner
 

twgbonehead

Vaping Master
ECF Veteran
Apr 28, 2011
3,705
7,020
MA, USA
Okay this is really interesting. I own a professional music studio, and I DIY my juice. With the untrasonic degassification, what frequencies are used? I have full range frequency spectral analysis programs on my studio's computers so I wonder if I could jerry up an old speaker's port hole to a short sterile tube to do this. It wouldn't be unreadable, as all speakers do are vibrate at different frequencies and move air to create sound, and the port hole on a subwoofer or studio monitor pushes out the reverberated air from the inside of the monitor.

Pretty much any vibration (even at much lower than ultrasonic frequencies) will do the job. (One poster on ECF used a "feminine entertainment device" and got very good results).
 
Pretty much any vibration (even at much lower than ultrasonic frequencies) will do the job. (One poster on ECF used a "feminine entertainment device" and got very good results).
Now that's a great idea for a thread, Smooth vs. Ribbed vs. Knobbly
Try telling my wife that it is experimental vape gear.
 
you mentioned surface area and degassification. would you think, have you tried, a thinner layer in a wide bottom dish? Do you think the container itself can play a role in the steeping process? most of us use 15ml or whatever the case a small surface area with a LOT of liquid beneath that is restricting oxygen with the exception of shaking. just saying....
Its not surface degasification, have a look at the video link, ultrasonic waves blast the gas out of the liquid from within
 

twgbonehead

Vaping Master
ECF Veteran
Apr 28, 2011
3,705
7,020
MA, USA
Hidden science behind normal and accelerated e-Liquid steeping.

We are all aware of the effect of steeping e-Liquid can improve its flavour and change its colour.

In this article I am attempting to describe the cause and effect systems involved in e-Liquid steeping and accelerated steeping from a scientific viewpoint.

There are two major processes involved in steeping e-Liquid

1. Removal of volatile components by evaporation and degasification

This process would include the removal of alcohol but is not restricted to alcohol, there are other volatile components used in the production of flavour concentrates that generally give off an astringent or chemical odour.

These process requires access to the atmosphere hence the need to remove tops from bottles

1a Evaporation – This is the same process as used in cooking to remove alcohol from wine.

1b Degasification – This is the sameprocess as letting a fizzy drink going flat

Both of these processes are accelerated by heat and increased surface area.

This is a critical first step many e-Liquids are hideous and un-vapeable before this process.

Without acceleration this can take a week or longer due to the viscosity of the liquid.

2. The development of complex flavour molecules.

Over time some e-Liquids especially custard / caramel or desert flavours darken over time

From observation this cannot be oxidation as it occurs uniformly through the liquid and does not require agitation of the liquid to occur.

It also cannot be caramelization as this does not occur below 110°C.

Maillard Reaction - Colour and flavour

What seems to be happening is a Maillard reaction commonly experienced by most people every day. The browning of bread, toast and potato chips these are high temperature examples. Medium temperature examples creating Dulce de leche and condensed milk.

Mallard reactions also occur at lower temperatures and contribute to the aging of wine and Balsamic Vinegar.

Maillard reactions get exponentially slower as they progress

This fits in with our observations of steeping e-Liquid, a golden colour may be observed in a couple of days however the full desired flavor and colour may take 4-6 weeks to develop.


The Maillard reactions will continue to progress over time, hence those almost black bottles of e-Liquid that are found at the back of a draw.

Accelerating the steeping process

Removal of volatile components by evaporation and degasification

a) Taking the top off the bottle.

Evaporation and degasification simply wont happen with the lid on (Think bottle of lemonade)

b) Shaking the bottle (Helps)

c) Stirring (Helps)

d) Whisking (Very effective)

c) Blending to a foam (Super Effective)

d) Ultrasonic degasification (Super Effective)

Video Showing Ultrasonic degasification
http://www.hielscher.com/degassing_01.htm

d) Heating to 40°C-50°C (Accelerates all of the above methods)

Maillard Reaction - Colour and flavour

a) Heating to 40°C-50°C (Maillard reactions go slower at lower temperatures)

b) Ultrasonic treatment (local extremes of temperature and pressure act as a catalyst)

In Practice

The image on the left was taken immediately after mixing the image on the right was taken 5 hours later

Steeping_zpsp3eux8si.jpg


60:40 VG PG 18% Nic 15% T-Juice Custard Concentrate

The e-Liquid was very vapeable the next day and is continuing to improve in the bottle.

Method used

a) Mixed liquid by weight directly into the blender cup.

b) Blended to a foam for 15 seconds remove lid

c) Placed into ultrasonic bath pre-heated to 50°C

d) 20 minuet ultrasonic cycle

e) 20 minuet rest

f) repeated (b) to (e) above six times

Then bottled into 50ml bottles

Storing after accelerated steeping.

Storing lid off in warm (room temp) draw or cupboard will allow any new volatiles to escape

This is less important as time passes.

The e-Liquid will continue its Maillard reaction gaining in richness, complexity and darkening
further.

There will be a point where you will not want the process to continue this is of personal preference.

This dictates how much you should make. As the Maillard reaction slows down most e-Liquids have a “Window of Niceness” lasting a couple of months.

The process can be slowed by refrigeration don’t freeze your liquid.

Quality and Issues

There is no quality related advantage accelerating the steeping of e-Liquid.

Heating some flavours may introduce unwanted cooked flavours.

If the acceleration process is overdone the “Window of Niceness” shelf life can be drastically reduced.

Full blown blending is impractical for quantities of less than about 100ml

Good old lid off in a dark place with a bit of a shake now and then will result in a perfectly steeped e-Liquid it is also far more predictable than accelerated steeping. It just takes longer.

As there are so many variables involved, you should always keep notes on how you
have steeped your e-Liquid along with the ingredients. You can then easily replicate your successes.


Joe Dyer

References

Wikipedia entry on Maillard reactions

http://en.wikipedia.org/wiki/Maillard_reaction

Description of low temperature Maillard reactions

http://cooking.stackexchange.com/questions/29926/what-temperature-does-the-maillard-reaction-occur


By

Joe Dyer


Very interesting stuff, Joe! This is a topic I have been very interested in, and there's not much solid info out there on the subject!

I have a couple of questions/comments:

1. You say "Don't freeze your juice". I have heard this repeated many many times, but have never been able to find a source or reason for this. The only thing close I could find was a statement by an employee of one of the flavor companies who said "You shouldn't have to freeze your flavorings, they will last for 6 months or more if refrigerated". Not a particularly definitive answer.
Do you know of an actual reason why storing flavored e-liquid in the freezer is a bad idea?

2. I'm not sure I would agree with you about the desirability of rapid evaporation of the volatiles, at least the ethanol. Over-agressive airing out of e-liquid does cause it to lose a lot of its flavor, at least in my experience. I have guessed that it's an issue of getting the flavoring molecules to separate from the ethanol, and re-attach to the other alcohols (PG and VG) and this takes time (but can be accelerated using heat, ultrasonics, vigorous shaking/stirring/frothing, etc). I worry that if you try to get rid of the alcohol too quickly, it will take a large percentage of the flavor molecules along with it. Also, once the alcohol and other volatiles are gone, I really wouldn't suggest storing liquids long-term open to the air.

3. I'm very interested in the idea that there would be a Maillard reaction going on. Are the right precursors present for such a reaction? Do the PG and VG act as the sugars in that reaction, and are the flavorings made of proteins suitable for such a reaction?
This does suggest, however, that if you're making a new batch of juice, and have an already-aged sample of the same juice, you could mix the two together and get the reaction to happen much more quickly, since the Maillard reaction is (believed to be, anyway) auto-catalytic. Would make for an interesting experiment, at any rate.

Thanks for taking the time to put this together! Looking forward to more info on the subject!
 

skoony

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why would you want to shake or stir the liquid?
it would just introduce more air into the mix.
the air introduced into the mix during the
manufacturing process is the primary reason
you have to let the product settle.
along with alcohol that may be in some of
the additives there's not much else going on.
depending on the mixture and viscosity after
a period of settling the juice becomes more
homogeneous. literally meaning the molecules
in the mix get closer together.
:2c:
regards
mike
 
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Sir2fyablyNutz

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will you pour the liquid in the cleaner or just set the bottles in there?

I put really hot tap water in the cleaner to the level of the liquid juice in the closed bottles. Then I set the timer for 480 seconds (8 minutes) hit temp (heat-TC) every other time and did 15 cycles (two hours worth). Then uncap the juice and let it breath in a cabinet for some time (until cooled plus a little).
 
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twgbonehead

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why would you want to shake or stir the liquid?
it would just introduce more air into the mix.
the air introduced into the mix during the
manufacturing process is the primary reason
you have to let the product settle.
along with alcohol that may be in some of
the additives there's not much else going on.
depending on the mixture and viscosity after
a period of settling the juice becomes more
homogeneous. literally meaning the molecules
in the mix get closer together.
:2c:
regards
mike

Mike,

That's one of the things that's still not well understood. The fact is, shaking e-liquid DOES cause it to steep more rapidly, as well as pretty much any other kind of mechanical agitation.

Closest to an explanation I can come to is this:
Ethanol is most commonly used for extracting food flavorings because it's very effective at penetrating cell walls, and drawing out flavorings from organic matter. It's a smaller molecule than PG (which can be used for extraction, but is not as efficient) and much smaller than VG (which is a pretty poor extraction vehicle, at least at room temps).
So now, we've got flavoring molecules, which are (loosely) attached to ethanol molecules. If you can break the flavor molecules off by agitation (and heating is another form of agitation) they will tend to re-attach to another alcohol molecule. But since the PG and VG (also alcohols) are also present (and in higher concentrations) the flavor molecules are more likely to re-attach to either the PG or VG.

Another surmise I have is that when you then let the volatiles evaporate out (slowly) that the "loose" alcohol molecules will be more likely to evaporate than the "stuck" ones (particularly if you let the vapor concentrate, such as leaving the caps on and only occasionally taking them off and exchanging the air). Therefore you can preferentially remove the un-attached alcohol, leaving more of the flavoring behind.

This could all be B.S. I am not a good enough chemist to really know the validity of anything I've said above, but I have given it a lot of thought, and this is the best explanation I've been able to come up with about what's really happening. That's why I am glad that Joe started this thread, since it hopefully will get the attention of more folks and perhaps with better brains than mine we can figure this out a little better.
 

skoony

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Jul 31, 2013
5,692
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saint paul,mn,usa
Mike,

That's one of the things that's still not well understood. The fact is, shaking e-liquid DOES cause it to steep more rapidly, as well as pretty much any other kind of mechanical agitation.

Closest to an explanation I can come to is this:
Ethanol is most commonly used for extracting food flavorings because it's very effective at penetrating cell walls, and drawing out flavorings from organic matter. It's a smaller molecule than PG (which can be used for extraction, but is not as efficient) and much smaller than VG (which is a pretty poor extraction vehicle, at least at room temps).
So now, we've got flavoring molecules, which are (loosely) attached to ethanol molecules. If you can break the flavor molecules off by agitation (and heating is another form of agitation) they will tend to re-attach to another alcohol molecule. But since the PG and VG (also alcohols) are also present (and in higher concentrations) the flavor molecules are more likely to re-attach to either the PG or VG.

Another surmise I have is that when you then let the volatiles evaporate out (slowly) that the "loose" alcohol molecules will be more likely to evaporate than the "stuck" ones (particularly if you let the vapor concentrate, such as leaving the caps on and only occasionally taking them off and exchanging the air). Therefore you can preferentially remove the un-attached alcohol, leaving more of the flavoring behind.

This could all be B.S. I am not a good enough chemist to really know the validity of anything I've said above, but I have given it a lot of thought, and this is the best explanation I've been able to come up with about what's really happening. That's why I am glad that Joe started this thread, since it hopefully will get the attention of more folks and perhaps with better brains than mine we can figure this out a little better.
your right of course. my point is the number one factor is getting the air out
because that's where most of the problem lies. heating or ultra sound
would not be re-introducing air into the mix.if any thing shaking would add water to
the mix which perhaps thins it out ever so slightly allowing for faster
evaporation of the excessive alcohol smell.
regards
mike
 
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twgbonehead

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Since ultrasonics are in such a high kHz range, and most monitors won't put out anything over 20-25k, I'm thinking going the opposite direction and going down to the low frequency range. Those reverberations would be easier to harness around the 40-70Hz range and would cause serious vibrations.

You win the interwebs for today! Brand new steeping mechanism:

Just pump up the bass, and store the bottles on top of your speaker cabs!


(If that doesn't get the FDA to ban e-liquids, I guess nothing will ;-)
 
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