Steeping Times and an Ultrasonic Cleaner Part III

[DejayRezme]

Would be really great to know what is going on precisely. Tasting is so subjective, if I take a couple of puffs then I will taste / smell less as with the first puff, just because my senses are getting used to it quickly. More theoretical knowledge and controlled tests would be great.

 

[mikepetro]

OK Folks, I will put this to bed once and for all. I myself am curious if the steeping effect is just from heat (ie potentially from the cavitation heat), or if the Ultrasonic vibration contributes as well.

So I am doing a controlled test.
Test Parameters:

• Mixed one 100ml batch of a Strawberry recipe.
• Filled two identical blue glass Boston Round Bottles to the same exact level, right where the threaded neck starts.
• Boston Rounds were approx 1oz. Put remainder of juice in a clear bottle as a control sample.
• Placed one bottle in a Crock Pot controlled to 135 F.
• Placed one bottle in the Ultrasonic controlled to 57C.
• Allow both batches to run for 3 hours, maintaining identical water levels in both vessels.
• Pour samples into a clear glass bottles for visual comparison
• Compare results against one another and Control Sample.

Here is the Crock Pot apparatus:

Here is the Ultrasonic apparatus:

Here are the 3 clear glass bottle, marked as to source:

Here is the recipe I used.

Strawberry Steep Test (36mg 100ml 50-50)

NIC-BASE SPECIFICATION
Nic1 RTS	10% in PG
DESIRED MIX SPECIFICATION
Mix Strength (mg/ml)	36mgl
Mix PG-VG Ratio (%)	50-50
Mix Volume	100ml
RECIPE VOLUMES
Nic1 RTS		36 ml
PG Essential Depot PG		4 ml
VG Essential Depot VG		40 ml
F1 TFA Strawberry Ripe	8%	8 ml
F2 VZ Strawberry	5%	5 ml
Saline	7%	7 ml

[/TR]

And the result is this:

 

[ValHeli]

thans so much for this Mike! I've been wanting to do the same test for months but never did get around to do it. I just figured to buy juices that didn't need steeping for my taste. LOL

The experiment you're conducting will certainly dispel some myths.


EDIT: it would also be beneficial to add plastic bottles to the mix to note the differences ( if any ) in how materials are affect by UC waves.

 

[Mowgli]

The test is still in progress, it will run until shortly after Midnight, I will post the results then.

....

 

[mikepetro]

thans so much for this Mike! I've been wanting to do the same test for months but never did get around to do it. I just figured to buy juices that didn't need steeping for my taste. LOL

The experiment you're conducting will certainly dispel some myths.


EDIT: it would also be beneficial to add plastic bottles to the mix to note the differences ( if any ) in how materials are affect by UC waves.

I work with 500 gallon Ultrasonics at work. I have been trained by Bluewave ( a leading manufacturer) on them. It is a pretty well established fact that plastic will absorb the ultrasonic to varying degrees, the softer the plastic the more it will absorb, rather than simply resonate.

 

[beckdg]

...

 

[ValHeli]

It doesn't seem to be as well established here in the vaping community and some believe there's no difference at all. You'd think that since glass is better that people should've invested a couple bucks more on glass bottles when they bought their UCs. This would be a good opportunity to show once and for all how much the difference is ( if any at all )

I work with 500 gallon Ultrasonics at work. I have been trained by Bluewave ( a leading manufacturer) on them. It is a pretty well established fact that plastic will absorb the ultrasonic to varying degrees, the softer the plastic the more it will absorb, rather than simply resonate.

 

[mikepetro]

It doesn't seem to be as well established here in the vaping community and some believe there's no difference at all. You'd think that since glass is better that people should've invested a couple bucks more on glass bottles when they bought their UCs. This would be a good opportunity to show once and for all how much the difference is ( if any at all )

You all can do your own test on this, I already know the answer from my Industrial Training, I dont need to do a trial to prove it.

Follow this link if you dont believe me.
"You should always use a stainless steel basket, as softer materials will absorb the ultrasonic energy. Never use plastic or other soft materials."

 

[mikepetro]

You all can do your own test on this, I already know the answer from my Industrial Training, I dont need to do a trial to prove it.

Follow this link if you dont believe me.
"You should always use a stainless steel basket, as softer materials will absorb the ultrasonic energy. Never use plastic or other soft materials."

Now if the results of this test show that heat was main factor in speed steeping, and that the Ultrasonic cavitation didnt contribute much (other than as a source of heat), then indeed there wouldnt be much difference between plastic and glass "for our application". Plastic does absorb ultrasonic energy, this is proven, but if it is only the heat that is benefiting us then who cares how much ultrasonic energy is absorbed.

Regardless, I wouldnt want to use plastic even in the Crock Pot. Plasticizers are known to leech out at elevated temperatures. Not sure I want them in my juice.

 

[DejayRezme]

Damn I recently bought a dozen 30ml needle cap bottles as the be all end all solution to DIY mixing and steeping without the need to decant multiple times. Are there any pipette caps for glass bottles with thin tip that you can use to fill up Kayfun style tanks? I only found some with bulge tips.

PS: Awesome experiment, really curious now. Thanks for taking the time. Can't wait for the result

 

[mikepetro]

Here are the results.

The two methods are VERY damn close. The Ultrasonic appears to be just a teeny bit darker, but not by much. I will check them again tomorrow in the sunlight. I will also taste them all tomorrow.

So..... it "appears" that the speed steeping effect of the ultrasonic may have been nothing more than exposure to the heat generated by the cavitation. A hot water bath in a Crock Pot gave very similar results. And crock pots are certainly a lot cheaper, though the mechanical thermostats in them tend to have a huge hysteresis effect. My Sous-vide controller took that variable out of this trial though.

I will report back again tomorrow, and also after one week of normal aging.

 

[mikepetro]

Damn I recently bought a dozen 30ml needle cap bottles as the be all end all solution to DIY mixing and steeping without the need to decant multiple times. Are there any pipette caps for glass bottles with thin tip that you can use to fill up Kayfun style tanks? I only found some with bulge tips.

PS: Awesome experiment, really curious now. Thanks for taking the time. Can't wait for the result

Not that I am aware of. I tend to mix and mechanically steep in glass beakers/flasks, then once the juice cools I pour it into my plastic Luer-lok bottles.

 

[Phone Guy]

Here are the results.

The two methods are VERY damn close. The Ultrasonic appears to be just a teeny bit darker, but not by much. I will check them again tomorrow in the sunlight. I will also taste them all tomorrow.

So..... it "appears" that the speed steeping effect of the ultrasonic may have been nothing more than exposure to the heat generated by the cavitation. A hot water bath in a Crock Pot gave very similar results. And crock pots are certainly a lot cheaper, though the mechanical thermostats in them tend to have a huge hysteresis effect. My Sous-vide controller took that variable out of this trial though.

I will report back again tomorrow, and also after one week of normal aging.

Awesome test Mike..... I'm curious to know how the end result tastes to you, I'm sure you're familiar with this juice recipe... So you will know what the end result should taste like, and what it does taste like after "time" steeping by it self. THIS IS A GREAT TEST.

 

[disco180]

This test is great but if you read the crockpot thread it was agreed that 150 f was the needed level for CP steeping, someone even in the thread tested nic levels afterwards and reported no nic level lost.

http://www.e-cigarette-forum.com/forum/diy-e-liquid/548175-more-uc-vs-crockpot-my-experience.html

 

[rowdyplace]

Wow! Subscribed to thread. This is a cliff-hanger!

Thanks Mike!!!

 

[mikepetro]

This test is great but if you read the crockpot thread it was agreed that 150 f was the needed level for CP steeping, someone even in the thread tested nic levels afterwards and reported no nic level lost.

http://www.e-cigarette-forum.com/forum/diy-e-liquid/548175-more-uc-vs-crockpot-my-experience.html

I hear you, but that wasnt the variable I was trying to test, "ultrasonic energy vs a simple hot water bath" was the variable I was testing so I stuck with a temperature I am comfortable with. The purpose of this trial was simply to compare the two methods and see if there was an appreciable difference with/without ultrasonic energy, all other variables being equal.

I am fairly confident that the aging effect will increase as temperature increases. The real question is at what temperature does nicotine start to degrade by a significant amount. Clearly it must degrade with temperature or Manufactures wouldnt recommend storage in the freezer.

The actual process temperature for speed steeping will be yet another trial someday, once I figure out the appropriate test for nicotine degradation. I have a nicotine titration test kit, but I am not sure that is the right test to determine nicotine degradation. I need to do some more reading on the matter.

I read of one individual who tested in "warm" water bath and measured a 16% drop in nicotine. However his results are fare from conclusive in my opinion. While the nicotine level testing was done to Lab standards, the actual mixing/cooking process wasnt. There was no Control Sample and the actual temperatures were not measured nor recorded.

Furthering my concerns about heat on nicotine is this article which essentially says that nicotine biodegraded significantly with the levels of heat found in a compost pile:

Biodegradation of nicotine in compost, which is composed of
sewage sludge and tobacco wastes, is an effective disposal method
for nicotine. The process of nicotine biodegradation was the most
efficient in the thermophilic phase.

Then there is this information, but he doesnt quote any verifiable references to substantiate the claim.

Various tests carried out at 40-80°C for up to 20 days appear to show no degradation of Nicotine in PG within a sealed container.
Breakdown of the chemical structure of Nicotine is noted to begin at approximately 300°C in an oxidising environment.

 

[bobalex]

Here I go with a couple of assumptions knowing full well the slippery slope that is.

I was under the assumption that non-tobacco juices didn't require the same steep times that tobacco flavors do. I've read of folks mixing up fruit flavors and vaping them immediately or at most a day or so later. When I made up tobacco juices (that's all I vape) the first time I had to wait 3-4 weeks before they 'arrived' at a vapable state. For the second batch I kept the bottles in hot water (emptying the cooled water and refilling with hot) , shook 'em like crazy every 15 minutes or so, and after hours and hours of that noticed very little difference. I still had to wait weeks for a good vape.

The first time I tried using my UC (cheap model, 3 minute timer) it took two days to get vapable juice. I wasn't constantly jumping up every 3 minutes to start another cycle so the needed number of 3 minute cycles (I lost count) was spread out over a couple of days. When I 'upgraded' to an 8 minute cycle UC I was more attentive and achieved a finished product after 30 eight minute cycles. These were 100% PG juices. When I started making 70/30 mixes I noticed adding the VG increased UC time by an hour.

So my assumption is that some flavors may need only hours of a hot water bath to mature while my tobacco flavors needed 240 minutes of heat and cavitation.

If I had the patience (I don't) and a slow cooker (I gave it to my daughter years ago) I might undertake a similar test to see how long it would take tobacco flavors to mature in a constant hot water environment. But that will never happen. Someday my UC will stop working and I can 'upgrade' to the UC model Danny uses.

Has anybody ever asked a commercial e-liquid manufacturer what steps they go through to mature their juices? A guy I asked kinda hinted they used something like a paint can shaker.

There. 2 assumptions and a hint.

Here's a real question. How long can nic be kept in the freezer before it degrades? With the FDA's new deeming regs (as written) we've got about 3-4 years before we have to start thinking along 'lifetime supply' lines.

 

[69CamaroSS]

Shade-tree juice shaker....3000 strokes/min will turn a clear juice completely white with aeration!!! Couple of blasts on this and let 'em sit a week.....done! ;-)

 

[DejayRezme]

Has anybody ever asked a commercial e-liquid manufacturer what steps they go through to mature their juices? A guy I asked kinda hinted they used something like a paint can shaker.

I've asked a german shop who mixes liquids and flavors from flavourart themselves what the suggested steeping times are and if they use any of the quick steeping methods. He answered (loosely translated)
"We are of the opinion that steeping is overrated and advice against any experiments for steeping acceleration".

Thanks bobalex for the thoughts, I guess this is most likely to be true. Different flavors might need different steeping methods. Besides tobacco flavors (who likely are also very different from one another) I've heard that custard flavors also need longer steeping. It would be awesome to find some chemists or perfumers who can illuminate the science behind this.

BTW, is RY4 from flavorart even considered a tobacco flavor?

View attachment 332204

Lol this is awesome!

 

[mikepetro]

Here I go with a couple of assumptions knowing full well the slippery slope that is.

I was under the assumption that non-tobacco juices didn't require the same steep times that tobacco flavors do. I've read of folks mixing up fruit flavors and vaping them immediately or at most a day or so later. When I made up tobacco juices (that's all I vape) the first time I had to wait 3-4 weeks before they 'arrived' at a vapable state. For the second batch I kept the bottles in hot water (emptying the cooled water and refilling with hot) , shook 'em like crazy every 15 minutes or so, and after hours and hours of that noticed very little difference. I still had to wait weeks for a good vape.

The first time I tried using my UC (cheap model, 3 minute timer) it took two days to get vapable juice. I wasn't constantly jumping up every 3 minutes to start another cycle so the needed number of 3 minute cycles (I lost count) was spread out over a couple of days. When I 'upgraded' to an 8 minute cycle UC I was more attentive and achieved a finished product after 30 eight minute cycles. These were 100% PG juices. When I started making 70/30 mixes I noticed adding the VG increased UC time by an hour.

So my assumption is that some flavors may need only hours of a hot water bath to mature while my tobacco flavors needed 240 minutes of heat and cavitation.

If I had the patience (I don't) and a slow cooker (I gave it to my daughter years ago) I might undertake a similar test to see how long it would take tobacco flavors to mature in a constant hot water environment. But that will never happen. Someday my UC will stop working and I can 'upgrade' to the UC model Danny uses.

Has anybody ever asked a commercial e-liquid manufacturer what steps they go through to mature their juices? A guy I asked kinda hinted they used something like a paint can shaker.

There. 2 assumptions and a hint.

Here's a real question. How long can nic be kept in the freezer before it degrades? With the FDA's new deeming regs (as written) we've got about 3-4 years before we have to start thinking along 'lifetime supply' lines.

You have a point there on the tobacco flavors. I dont use them so I am ignorant as to their characteristics. I have seen through all of the posts though that they can be challenging.

As to fruit flavors needing speed steeping, some definitely benefit. Anytime a juice changes in color as it ages I figure that the UC/CP will benefit it. Strawberry, dill, some berries, and bakery flavors all fit that category.

The information I have seen on long term nic storage said that after 2 years in the freezer there was only about a 2% reduction in strength. Again though, it is sort of anecdotal evidence as I havent seen a bonafide properly controlled trial.

If the FDA thing turns out as currently written, I will buy some 99.7% nic from the darkside, then as needed dilute some by 75% and do a nic titration to determine its current strength, and mix from there. Already tested my sources and I am confident in them.

I have learned how to build my Mods, learned how to make my own juice, now I need to learn how to build a decent atty. Self sufficiency is my goal. If the market dries up I need to know how to fend for myself.