Steeping Times and an Ultrasonic Cleaner Part III

[mikepetro]

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.

I get it, I think. This would allow us to calculate the "rate" of decomposition.

So now to figure out an apparatus in my home that will accurately maintain 194 F for 48 hours. I believe my Souse-Vide controller and an electric tea kettle would do it. Hmmmmm.....

Alas I only have one temperature controller so my tests will need to be sequential.

 

[mikepetro]

However if those test kits are 10% inaccurate that could be why Im not seeing it.

I wouldnt say 10% inaccurate. They are accurate "within" 10%. So a given sample could be dead nuts on the money, or it could be as much as 10% off, or anywhere in between.

To increase the accuracy of your test, use a higher nic concentration, and/or a larger sample size. The more HCL you have to use, the more mathematically accurate (higher resolution) your test will be. If you have a 1ml syringe laying around, use it for the last ml of HCL, this will also allow a higher resolution of accuracy. Bulk add the first few ml with a 3 or 5 ml syringe until the solution turns green, then switch over to a 1ml syringe to turn it yellow.

If it becomes faint of color in the blue/green/yellow transition, making the color change hard to see, simply add some more bromothymol blue and it will make the color more vivid without affecting the test results at all.

 

[mikepetro]

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.

I get it, I think. This would allow us to calculate the "rate" of decomposition.

So now to figure out an apparatus in my home that will accurately maintain 194 F for 48 hours. I believe my Souse-Vide controller and an electric tea kettle would do it. Hmmmmm.....

Alas I only have one temperature controller so my tests will need to be sequential.

OK, so how is this for a trial?

• Make a 300ml batch of juice at roughly 4% (40 mg) nic
• Label 10 30ml Boston Rounds. 1 each with: Control Sample, 150F/2 hours, 4, 6, 8, 10, 12, 24, 48 hours, and 1 with 194F/48hours.
• Cook, cool for one hour, and test the 194 F sample
• Place all 8 150F samples in a hot water bath and cook each for the stated amount of time.
• Allow each to cool for one hour and test.
• Test the room temperature Control Sample
• Plot a curve of the results
• Each test would be to the same protocol as before. I.e. three 5ml tests of each sample and then average the result.

Theoretically this would give a degradation curve at 150F. Then, once you know the degradation curve you could compensate for the potency loss of heat steeping but increasing the nic in your recipe by X amount. Get the benefits of heat steeping at the potency you desire!

I am guessing that the 194 F sample is just to let us know the extreme. The eight 150F samples should plot a nice curve that covers the actual region of water-bath time that most people are using.

Question: Does the temperature of the sample being tested affect the results? In other words do I need the cool down period?

Anybody know of a good source of 0.1N HCL by the gallon?

 

[rowdyplace]

OK, so how is this for a trial?

• Make a 300ml batch of juice at roughly 4% (40 mg) nic
• Label 10 30ml Boston Rounds. 1 each with: Control Sample, 150F/2 hours, 4, 6, 8, 10, 12, 24, 48 hours, and 1 with 194F/48hours.
• Cook, cool for one hour, and test the 194 F sample
• Place all 8 150F samples in a hot water bath and cook each for the stated amount of time.
• Allow each to cool for one hour and test.
• Test the room temperature Control Sample
• Plot a curve of the results
• Each test would be to the same protocol as before. I.e. three 5ml tests of each sample and then average the result.

<<snip>>

Anybody know of a good source of 0.1N HCL by the gallon?

I called WL and they do not package this in gallons - the 500 mL is their largest item available. Hydrochloric Acid 0.1N (HCl) - 500ml (16oz) And, you still will need the nic/pg/vg...

I will chip in and pay for one of these 500 mL bottles of Hydrochloric Acid 0.1N (0.05M).

I'm sure we can get 7 other volunteers to do likewise.

Let us know if you want our assistance in this matter. Many of us appreciate your efforts...

 

[mikepetro]

I called WL and they do not package this in gallons - the 500 mL is their largest item available. Hydrochloric Acid 0.1N (HCl) - 500ml (16oz) And, you still will need the nic/pg/vg...

I will chip in and pay for one of these 500 mL bottles of Hydrochloric Acid 0.1N (0.05M).

I'm sure we can get 7 other volunteers to do likewise.

Let us know if you want our assistance in this matter. Many of us appreciate your efforts...

I appreciate the offer of assistance. I wasnt really lobbying for it, but I wont turn it down either.

I really only need about 1 liter of HCL to do the testing. 740ml to be exact assuming no waste or "do-over" tests, but with 30 tests being performed I expect there will be a few that get discarded and done over.

I have enough nic in the freezer to make over 25 liters of 100mg concentrate (no I am NOT a vendor). So I can contribute the nic, no problem. I have about a gallon each of pg and vg so that isnt a problem either.

Really the bromothymol blue, the HCL, and some time is all I need to accomplish this test regimen.

 

[buffaloguy]

I think you can buy those larger sizes of hydrochloric at pool supply stores. As well as bromothymol. Although I havent been to a pool supply place since I was a teenager. And thanks for the tips on testing.

 

[mikepetro]

I think you can buy those larger sizes of hydrochloric at pool supply stores. As well as bromothymol. Although I havent been to a pool supply place since I was a teenager. And thanks for the tips on testing.

The stuff that most pool supply places carry is 0.12N HCL which is about 20% stronger. While the math to calculate nicotine using this strength HCL exists (and is indeed used by some nic test kits) using the 0.1N is more accurate (ie higher resolution).

 

[Phone Guy]

So has anyone tested the samples Mike steeped? I'm curious to know the end results.

 

[mikepetro]

There was about 3ml of each of the three samples left over, a guy at work really liked the remnants of the three mixed together!

 

[rowdyplace]

That sir, was a very diplomatic dodge. YOU sure you are not in Marketing??

(You can get fired in Engineering for doing the same thing that will get a Marketeer a bonus!!)

 

[RocketPuppy]

So has anyone tested the samples Mike steeped? I'm curious to know the end results.

Haven't received yet, but I imagine the post office is getting bogged down with people sending Memorial Day packages and letters to their kids.

Damn! My sarcasm font doesn't work on tapatalk.

 

[DVap]

OK, so how is this for a trial?

• Make a 300ml batch of juice at roughly 4% (40 mg) nic
• Label 10 30ml Boston Rounds. 1 each with: Control Sample, 150F/2 hours, 4, 6, 8, 10, 12, 24, 48 hours, and 1 with 194F/48hours.
• Cook, cool for one hour, and test the 194 F sample
• Place all 8 150F samples in a hot water bath and cook each for the stated amount of time.
• Allow each to cool for one hour and test.
• Test the room temperature Control Sample
• Plot a curve of the results
• Each test would be to the same protocol as before. I.e. three 5ml tests of each sample and then average the result.

Theoretically this would give a degradation curve at 150F. Then, once you know the degradation curve you could compensate for the potency loss of heat steeping but increasing the nic in your recipe by X amount. Get the benefits of heat steeping at the potency you desire!

I am guessing that the 194 F sample is just to let us know the extreme. The eight 150F samples should plot a nice curve that covers the actual region of water-bath time that most people are using.

Question: Does the temperature of the sample being tested affect the results? In other words do I need the cool down period?

Anybody know of a good source of 0.1N HCL by the gallon?

I'd simply quench the samples coming off of the heated bath in cold water, shake and test.

Try this for the acid. a quart (945 mL) of 2.5N hydrochloric acid for $25.99 including shipping. Simply dilute precisely 160 mL of the acid to a final volume of 4.0 liters with distilled water. Enough to make almost 24 liters of 0.1N hydrochloric acid, that's over 6 gallons.

Edit: 2.5N hydrochloric acid is about 4.8 times more dilute than the super concentrated stuff at 37% in water (which is about 12N). Doesn't fume nearly as badly and isn't quite so nasty as the concentrated stuff, but it's still worthy of respect. Can't get hydrochloric acid solution at more than 37%, that's all the hydrogen chloride gas that will dissolve in water.

On an unsolicited practical note, there are times when a chemist will prefer sulfuric acid, times when a chemist will prefer hydrochloric acid, and times a chemist won't care which is used. The nice thing about hydrochloric acid is that it can be added to something to perhaps produce an alkaloid salt, and then once the water is removed, the hydrochloric acid is also gone since it's native form is a gas. With sulfuric acid, once you've evaporated the water, you're left with a residue of non-volatile concentrated liquid sulfuric acid... and the stuff is vicious.

 

[rowdyplace]

Danny45 - Go check your shrubs and ditches for the mailman. According to official US Guvment records, it's there!

RocketPuppy - Leave HappyHour a little early today, yours should be in your box.

 

[rowdyplace]

MikeP - Check your PM!

 

[mikepetro]

Well........

Thanks to the lobbying efforts of Rowdy, and the generosity of Wizard Labs, I now have enough reagents coming "free of charge" to perform this testing.

Exciting stuff!

 

[dannyv45]

So has anyone tested the samples Mike steeped? I'm curious to know the end results.

Samples are "out for delivery" so they should be there by the time I get home from work.

 

[dannyv45]

Danny45 - Go check your shrubs and ditches for the mailman. According to official US Guvment records, it's there!

RocketPuppy - Leave HappyHour a little early today, yours should be in your box.

Just need to look in the flower bed, roll the postman out of the way and they should be right there Although by the time I get home from work the postman should be sobered up enough to leave under his own power

 

[buffaloguy]

Well........

Thanks to the lobbying efforts of Rowdy, and the generosity of Wizard Labs, I now have enough reagents coming "free of charge" to perform this testing.

Exciting stuff!

Thats awesome and another reason to add on to the list of why I keep doing business with them. You've hooked me into these new tests Mike, cause it'll definitely answer the questions I had relating to how heat impacts nic strength at different lengths of time and what adjustments would be necessary if any to compensate.

 

[dannyv45]

Well........

Thanks to the lobbying efforts of Rowdy, and the generosity of Wizard Labs, I now have enough reagents coming "free of charge" to perform this testing.

Exciting stuff!

That is excellent news. Way to go guys

 

[Blueser]

Outside of 4-5 folks there seems to be little or no interest at what heat point nic begins to degrade or the entire UC/CP debate. Maybe a lot of folks just aren't in a big hurry to heat force their mixes into maturity but rather prefer to let their mixes age/blend naturally with time or else are satisfied with their juice freshly mixed.

I do wonder what have you actually accomplished if after all this testing that you find a few degrees over a certain temperature the nic degrades a certain amount. I also wonder if the differences in nic extraction methods and the quality of the nicotine used would not have a bearing on test.

Take the new on the scene VT nic for example. Folks who were using WL nic are now stating that there is no comparison between the quality of the two and are finding little to no need to even age/heat their mixes with the VT nic. This all makes me think that a little or lot of nic degradation might be a good thing, especially if it helps lessen the foul/metallic taste of some nicotine or vice versa with a higher quality/clean nicotine that heating would be at all necessary.