Steeping Times and an Ultrasonic Cleaner Part III

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disco180

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In addition to the nicotine degredation (suspected ?) from hot steeping your juice, dont forget that many flavoring vendors have used acetion and acetyl propionyl to replace diacetyl. Take a look into homebrewed beer, all you need to do is heat a sample to 150 degrees Fahrenheit to cause the formation of diacetyl. *I think* diacetyl is formed from acetoin after heating... So in general, using a crockpot, or the heater on my UC is out!

I'm just assuming that for everyone that uses a crockpot, you are breaking down the nicotine, and creating toxic chemicals in your juice. I am no chemist...

Pseudo-Science at its finest!!!!!!!
 

mikepetro

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Don't most of our flavorings come from the food industry?

Wouldn't cooking, making candy, and baking have the same negative effects on the chemicals and therefore on us?

All of these meet or exceed 150° F.

I wouldnt count on all vaping flavorings as coming from the food industry. Some are from food, some are not. For example I dont know of much call for tobacco flavoring in food. Care for some RY4 in your cappuccino?

Even in the food industry flavorings are made/marketed to specific sectors of the Industry, such as candy, bakery, beverages etc. Thus, those flavors are exposed to very specific processes. Think about Kool-aid, it is not typically exposed to heat, can it handle it, who knows, but it wasnt designed for heat Chocolate flavorings are not designed to go above the tempering temperature, certainly not above 150F. Also look at TFA, they originated from the perfume industry. While their flavorings may be considered food safe, their approach (and most of their chemicals) was from olfactory origins. They even express the safety of their flavors in ppm(/t), as in not to exceed XX ppm.

Also keep in mind that a major portion of our flavorings come from China, where even their baby-formula isnt necessarily food-safe!
 

DejayRezme

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    I'd be interested about how many "tobacco" flavorings actually taste anything like any kind of cigarette, cigar or pipe. I'm pretty sure my RY4 (from flavourart) has nothing to do with cigarettes. I love RY4 but I thought that "tobacco" flavor for vaping generally only means something like a rich, complex and/or somehow earthy flavor. Besides the real "tobacco leaf extraction" flavors all the tobacco flavors of flavourart afaik do come from the food industry. Sorry if this is a bit off topic but I'd be interested in how other people who like real tobacco smoking flavor see the tobacco juices and if there is anything you could give a try. And what it is about tobacco flavors that makes them require steeping. Judging from the color, my RY4 seems to be one that doesn't really require steeping but that one might be special. But I don't have much experience.
     

    RocketPuppy

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    Our precious cargo was personally handed to a uniformed USPS employee at 2:45pm today in Birmingham, Alabama 35242.

    Bottled in glass, sealed in plastic, padded with Styrofoam P-nuts, enclosed in cardboard, sealed with scotch tape, they should be good to go.

    What an outrage! Phooey!!! Are you telling us you didn't use Argon gas to eliminate the poisonous oxygen contaminating the juice? Did you at least use vacuum sealed containment bags? The horror!

    =)
     

    RocketPuppy

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    In addition to the nicotine degredation (suspected ?) from hot steeping your juice, dont forget that many flavoring vendors have used acetion and acetyl propionyl to replace diacetyl. Take a look into homebrewed beer, all you need to do is heat a sample to 150 degrees Fahrenheit to cause the formation of diacetyl. *I think* diacetyl is formed from acetoin after heating... So in general, using a crockpot, or the heater on my UC is out!

    I'm just assuming that for everyone that uses a crockpot, you are breaking down the nicotine, and creating toxic chemicals in your juice. Even just using the UC for 10-15 minutes will raise the temperature of the bath 10 or 20 degrees, so a gentle heat along with the UC is enough for me.

    I also wonder about other chemical reactions with various flavors mixed together when hot-steeping... I am no chemist...

    The tests were done without flavor additions.
     

    DVap

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    That would be accurate.

    THE HCL Titration tests for alkalinity/ph only and cannot differentiate nicotine from any other ingredient. Various additives like flavoring, lemon juice, saline, vinegar etc "can" alter the ph and/or alkalinity and skew a HCL titration result with respect to nicotine alone.

    For a HCL titration to give accurate results you need to do it on nicotine base, ie nothing other than pg/vg added.

    I've tested many flavored liquids and found that, generally, they titrate quite close to the actual nicotine level. Obviously, acidic or basic ingredients will affect the result, but in practice, I've rarely come across liquids containing them. That being said, when I first published the nicotine titration method here back in 2009, I was pretty insistent that it was intended for the testing of nic/PG or nic/VG mixes. The tests from Wizard Labs and others are all based on my method, and I believe each test supplier warns of the possible skewed results that might be obtained with flavored liquids.
     

    rowdyplace

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    What an outrage! Phooey!!! Are you telling us you didn't use Argon gas to eliminate the poisonous oxygen contaminating the juice? Did you at least use vacuum sealed containment bags? The horror!

    =)

    These were precautions taken to protect it from the routine handling by the USPS. The juice is on it's own...

    PS...your late again...Where are the cookies??
     

    RocketPuppy

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    These were precautions taken to protect it from the routine handling by the USPS. The juice is on it's own...

    PS...your late again...Where are the cookies??

    Life right now: Senior class advisor, baccalaureate speaker, department chair, interview new teachers for next year, write baccalaureate speech, finish master's dissertation, give and grade finals for my own students, etc, etc, blah, blah, blah, no one cares =)

    In two weeks, my life can start again, and you will be rewarded.
     

    DVap

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    I'm giving this all a bit of thought and I'm not sure about the oxidation products. The primary metabolites of nicotine are cotinine and nicotine-n-oxide, but mostly cotinine. Nothing more happens to nicotine-n-oxide and it is excreted unchanged. If I understand correctly, it can be reduced back to nicotine in the body (now we're talking thermodynamics and reversible reactions and that gives me a headache). Both nicotine and cotinine are metabolized primarily by the CYP2A6 enzyme (nicotine much more quickly than cotinine, thus it's shorter half-life). So nicotine ends up as cotinine and nicotine-n-oxide can either be excreted unchanged or reduced back to nicotine (thus ultimately being metabolized to cotinine and onward to 3'-hydroxycotinine which is ultimately dumped into urine). Since CYP2A6 activity can vary between individuals, clearance of nicotine can be a variable affair with the half life varying more or less on an individual basis.

    This probably has little to do with what happens to a nicotine solution when heated since in this scenario, the CYP2A6 enzyme is not part of the picture.

    Of what use is all this? Dunno, mostly thinking out-loud and typing at the same time.

    If we look at a room temperature nicotine solution at 70F versus a nicotine solution at 150F, what can we easily gather about the kinetics of nicotine oxidation in a non-biological system? The first thing we need to do when dealing with kinetics is to get the temperatures onto an absolute scale and for this, we use the Kelvin scale. The Kelvin scale starts at absolute zero (-273.15C) and goes up from there corresponding to the graduation found on the Celsius scale. So if we look at the freezing point of water (0 C), it corresponds to 273.15 K. Room temperature (70 C) corresponds to ~21C and 150F corresponds to ~65 C. Or on the absolute Kelvin scale, a room temperature solution would be ~294 K and a 150F solution would be ~338K. Absolutely speaking, the 150F solution is about 15% "hotter" than the room temperature solution.

    We know that a nicotine solution at room temperature is stable day to day (but can slowly oxidize) and we have tests to suggest that a number of hours at 150F might result in a noticeable oxidation of nicotine. With kinetics, we can see a couple things happen. In some cases, nothing happens up to a given temperature, but once that temperature is reached, a reaction will proceed quickly to completion. In other cases, the reaction occurs more slowly or more quickly depending on the temperature, but there is not necessarily a "critical" temperature at which the reaction begins and goes like gangbusters. Nicotine appears to behave like this under the temperatures we're looking at here (though get it hot enough and it will likely rapidly decompose like in the first case).

    Since we're not heating the nicotine in an enzyme affected biological system, we're looking at straight kinetics (well, the enzyme system is kinetics too, but the enzyme provides an alternate "assisted" kinetic route). Since I'm not sure offhand what exactly the heat induced oxidation products are, we're also not sure how these oxidation products behave in an acid titration.

    So we're left with fairly simplistic testing opportunities. A control solution of nicotine in PG at room temperature will be basically unchanged after a week. Testing here suggests that a nicotine/PG solution held at 150F might oxidize at around 1% per hour (if I remember the results correctly). My approach would be to make 4 identical solutions and leave a control solution (A) at room temperature and leave another solution (B) at 150F for 8 hours and another solution (C) at 150F for 48 hours. The last solution (D) would be left at 90C (194 F)(363 K) for 48 hours. We would expect the determined degree of nicotine loss (assuming some or all of the oxidation products don't titrate) to be A < B < C < D. C should be perhaps approximately 6X more affected than B (but perhaps not exactly since the rate of oxidation might decrease over time with decreasing nicotine concentration.

    Anyway... maybe more than folks wanted, and possibly some erroneous assumptions here... I've definitely not researched any of this beyond a surface glance.
     
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    vgnut

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    But before I drift I just wanna say the Heat Steeping Experiments are downright intriguing.

    V4L sent me a ton of stuff to review months ago and I Finally Finished so ... I want to share with my Steeping DiYers.




    Nice work! Although I was hoping for one of those 50's type ......... ads where the guy smokes a joint and then puts a shotgun in his mouth... :). vaping kills!
     

    buffaloguy

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    I have to say Mike your explanation and testing methods definitely seem sound. You have actually helped me look at the information I already have seen in ways I haven't considered in some cases.

    I never ever mind being wrong if Im being educated! Thank you.

    When Im testing at home I am doing a before and after heating comparison of the nic and vg base from the same lot #. I always track my lot #'s from bottle to bottle. Just habit in case WL ever recalls something. One big thing for me is consistency of results in my mixing and I have my methods that work for me to replicate the recipes I make so there are no variations from batch to batch. It works too. Knowing if my base is off nic wise after heating has always been a part of that. However if those test kits are 10% inaccurate that could be why Im not seeing it.

    Im stll wondering on the question of whether less time than 8 hours at 150° would help to minimize the nic loss. As I said I only typically do 4 hours. I guess it stand up to reason that it would be less nic lost with a shorter time frame, but Im curious as to how much? Do you have thoughts on this?

    Thank you for taking the time to help explain and put up with my shock... and questions. Its commendable work you are doing and I truly do appreciate it.

    These were strong words my friend. Nothing in your response backs up your contention.



    It is a good "rough" test that is essentially a commercialized version of DVap's original method published back in 2009, which DVap himself (an accredited Chemist) says is only accurate to within 10%. The margin of error of that test kit/method is greater than the amount of potency loss I measured so you cant reasonably use that test kit as a basis for saying "my tests are wrong". I estimate the accuracy of my testing apparatus at +/- 2%, combine that with averaging three tests together and I estimate the accuracy at better than +/- 1%.

    At the smaller sample size used, and by applying HCL with a syringe rather than a burrette, it is considerably less precise than the method I am using. My larger 5ml sample size is simply mathematically more accurate because it requires more HCL to protonate the nicotine. Using a syringe for applying drops of HCL introduces more variability than a burette. Lets face it, a burrette with .1ml markings is much easier to read, and more precise than drops from a 3ml syringe. I have the Wiz Labs kit, but I didnt want to accept +/- 10% accuracy when diluting very strong (ie pure) nic concentrates, so I acquired the burrette and magnetic stirrer to achieve better accuracy.


    IMHO, unless you test a heated sample, and an unheated sample, from the exact same "Lot", on the same day, using the same test method, then you dont have a conclusive test. Given the amount of judgement involved interpreting color, and measuring with a syringe, a single test can be misleading, best practice dictates doing multiple tests to ensure repeatability.




    Actually my testing does "jive" with this test, in fact he showed a larger loss of potency than I did! I agree, his results are far from conclusive, especially since there was no uncooked control sample (from the same batch of juice) to establish a baseline. However, even if we assume his test is accurate, if you do the math he is demonstrating over a 16% loss of potency! "a drop of .1% or 1mg/mL of nicotine" divided by the original "0.6%(6mg/mL) nicotine" is a 16.6% loss of potency.


    As you said, the spectroanalysis might not represent nic strength, unless nic is represented by one of the wavelengths. It is notable that the transmittance is lower across the whole spectrum for the heated sample. So if nic is represented by a specific wavelength, it would be lower than the untreated samples.

    Yes, it was Kurt who did the coil testing. Not really relevant to steeping though.



    I hear you, but to me this is purely anecdotal. "So and so said they got this" doesnt really prove anything without hard data to back it up. Were they employing proper methodology in their tests? Were they being objective? Were they testing juice that had other additives that might have altered the alkalinity?

    What I was trying to do was apply a "best practice" analytical approach to definitively answer some of these questions one way or another. I really didnt care what the results were, I just want to know the facts, and cut through the myth and the anecdotal.

    I am an Engineer, not a Chemist, but my training tells me that a proper test should always include
    • A control sample to establish a baseline for whatever method of testing is used. I.e. a sample from the exact same lot that has not been processed or altered that can be subjected to the exact same testing method. This establishes a "baseline" to which the other results can be compared.
    • Testing multiple iterations of the same sample ensures the repeatability of the test and eliminates possible testing/human error.
    • The best test equipment you can afford. The higher the accuracy of your testing equipment, the more dependable your results.
    • Employing "best practice" techniques in your testing.

    I documented employing all of the above in my blog post, I stand behind my results.........
     
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