Test: Freezing liquid

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CZEdwards

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May 27, 2009
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I just got an order of 36 mg/ml from Eastmall and it came in 10 ml bottles. I happen to have a number of bottles now of 36 mg, so I tossed one in the freezer (set at 0F/-18C). I'll get it tested next week. I will post about the efficacy of this.

Test parameters:
1. Does niquid freeze? (Funny enough, this hasn't been answered yet.)
2. Does it melt without noticeable damage to a) appearance (color, clarity, viscosity)? b) nicotine content? (testing by HPLC, comparing unfrozen sample to frozen and defrosted sample.)
3. Can the bottles withstand freezing?

Anything else I should look for? (In terms of long-term storage, if freezing damages the liquid, that will be obvious after a few days in the freezer, and storage at -18C is usually enough to prevent degradation.) The HPLC report will give me a content analysis of the two samples (i.e. I can see if those two samples contain anything besides nicotine, distilled water, PG and glycerol (glycerine)) though two data points do not prove anything.

(Yes, I know having access to a high performance liquid chromatograph lets me play with a piece of equipment most people don't have, and yes, I'd LOVE to test a sample of every niquid I can get my hands on, but I'm getting these two samples tested because somebody in the organic chem lab owes me a huge favor (of the get up in the middle of the night and drive 40 miles in pouring rain type) and won't likely happen again. I'm trying really hard to interest one of our shared brand new grad students in the testing project, and if so, I'll let this community know it's happening, but if I do get someone interested, I can't publish results until after zie publishes in peer review and that won't be soon. I'm also working on getting another grad student interested in testing blood levels of nicotine, cotinine and free dopamine in smokers, non-smokers, NRT users and vapers, but funding that study is going to be painful -- our normal funding sources won't pay for it, we'd need at minimum 50 of each test subject and a minimum 2 blood draws each (because the spit tests don't show levels, just presence of cotinine), and getting our alternative funding sources (drug companies) interested is going to take work -- so don't expect much.)
 

sparky_ahs

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Jul 31, 2009
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This wasn't covered in your post. For the sake of a control are you going to split a single bottle into two groups one frozen and one not? I know its a bit tedious but if you are going to be using a HPLC with very accurate numbers then the two different bottles from the same shipment may also be from different batches ie. one is 36.4 mg and the other is 35.9mg nic to start out with. All factories have some margin of error.
 

CZEdwards

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Sparky -- ack. Didn't think about that. Yep. I just pulled a second bottle, divided it, and threw half in the freezer. (Dam mitt, this is what I get for designing experiments while sleep-deprived.) Worst case, I have a slightly off bottle of liquid.

I could only get two samples (for more, I'd have had to have driven a lot further than 40 miles... our machines' time is pretty heavily scheduled) so the data points will be coming from one bottle. Not great, but it is a completely random sample, which counts for something.

Stevo -- have you turned an elephant into a vaper? (Not many creatures have 220 kg of blood... even steer only clock in at about 45 kg) :) And yes, I know it has to be much colder to freeze solid, but I'd say only 10% or so of vapers have access to the type of cold storage that would actually freeze the stuff, while almost all of us have access to a household freezer. *THAT* I did take into consideration.

I am working on getting the studies at least started, and I've got one of our Emeritae interested (which helps). Unfortunately, with funding tight (even here at CU, and we pulled in the grants this year) all over, and no clear financial interest obvious (I know, but tell that to funders), getting the bucks is tough.
 

DVap

Nicotiana Alchemia
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Aug 26, 2009
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If it does not freeze it may be the cold will preserve it longer?
I wonder what it's like to vape really cold liquid?
Hot coil, cold liquid...
may turn into a Torvapor!

It will not freeze.

Keeping things cold is quite useful when you're looking at spoilage issues and microbes as the responsible parties. It's also quite useful when you're looking at losses via volatility. It's perhaps a bit less useful when you're looking at oxidative breakdown. On the absolute temperature scale, the difference between 0°C and 20°C is the difference between ~273°K and ~293°K. Not that great a difference actually, so it may not help much, but it shouldn't hurt either.

Vaping cold liquid? Seems like the atomizer will have to work harder and the battery will run down faster, though the volume of liquid that can fit into a cart will quickly warm up so it probably makes little real difference.
 

DVap

Nicotiana Alchemia
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Solid? Holy spit.

Do you know what the ratios were?

I know that VG/Water can drop the freezing point well under -18°C, and I wouldn't expect this from just PG or PG/Nicotine.

Are we looking at a mix of PG, VG, and nicotine? Perhaps the VG's effect in a non-aqueous system is to raise the freezing point since it's not like with water where VG does it's hydrogen bonding thing with water to disrupt the ability to crystallize.

I'm not quite ready to turn in my chem degree, but I might talk to the university about getting me a refund! ;)
 

Thatdamncat

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Aug 29, 2009
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I'm not surprised it froze. A google search of PG probably made some of you think that it would not freeze. However, the addition of water disrupts the H-bonding of PG and greatly raises the freezing point. Likewise, water has the same effect with the bp. Pure PG would probably not vape at all. Also, PG and water are completely miscible, so a physical state change like freezing shouldn't affect the quality of the soln. and might be a great way to store long-term. The only unknown for me is the flavorings. I'll be interested in your results.
 
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