Houston, we have a problem...BE nic titration results

[Kurt]

I saw a post here that suggested one need only test the ingredients. I think this case shows clearly that this would not be sufficient; one must test the final result.

It is quite feasible that the present situation was the result of incomplete mixing and only sampling the finished batch would show up the problem.

+++

To avoid the possibility of malfeance, the independent testing body along the lines Rolygate suggested would need to obtain samples in a way that was completely obscure to outsiders.

Hopefully such a body arises soon.

+++

@ Kurt - do the home test kits allow for neutralising / setting a baseline with regard to any acidic additives. Is this automatic or mentioned in the instructions, or would it require additional steps?

No, since added acidic ingredients that lower the pH would actually create a partially titrated nic, thus the indicator titration would show less total nic than was actually there. This is why I went with the curves. Its is more involved, but nic salt content would be accounted for based on the initial pH, the volume at first inflection, and volume and pH at second inflection. The math is involved but not difficult, just algebra.

It seems however that BE uses only freebase nic for sold liquids. That is evident in these curves. If it wasn't the case, and something like citric acid was added (example Vermont Vapor 35 mg VG), then the initial pH would be closer to 8 (pKa of the salt) rather than 10+ which is what I am seeing with BE and MFS. This whole thing was spawned from my wanting to know what the freebase/salt ratio was for BE, since it smelled less and hit less than MFS at the same conc. I sent repeated emails to them to find out. Not a word of reply, like I didn't exist. I tried to estimate with pH paper, since at the time my resources were quite limited, and that showed me it was far more freebase than VV, but not quantitatively. I knew the only way to see this was a pH-curve, as others in the Nic forum have done, but I didn't have the equipment then. I do now. So this was why I originally did my 100 mg BE, not because I doubted the nic content, but I wanted to see the freebase/salt content. Little did I know that it was actually less than 1/2 the nic content sold, and thus opened the floodgates.

 

[kinabaloo]

I concur for the need of such a body, but the overwhelming question in my mind is regarding chain of custody. How would such a body go about achieving a legal chain of custody without the supplier knowing of such? I do understand that analyses can be performed sans chain, but to ensure such findings have the maximum effect, such a chain would really be necessary in my opinion.

I was thinking that samples would be obtained via anonymous buyer - but yes, that's not as easy as it sounds.

Depending on the scale or nature of any error found, it might be sufficient to first warn the company and give them time to put things right before going public (perhaps issuing a recall if necessary). At some point a name and shame would ensue. I'm not sure the body would necessarily want to get into legal battles, but these could be initiated by the supplier and then the chain issue would arise. So perhaps you are right to an extent at least. It's not such a simple thing to do and might require substantial financial backing.

 

[kinabaloo]

No, since added acidic ingredients that lower the pH would actually create a partially titrated nic, thus the indicator titration would show less total nic than was actually there. This is why I went with the curves. Its is more involved, but nic salt content would be accounted for based on the initial pH, the volume at first inflection, and volume and pH at second inflection. The math is involved but not difficult, just algebra.

I just wanted to establish that simple home kits may not be accurate in some cases. Because there is likely to be much interest in them. Some extra knowledge and maths would be required to get accurate results in cases when acidic additives are present, if possible at all just those kits and other equipment or chemicals.

 

[redgirl]

Wow, just wow. So glad you did this, Kurt. Thank you for stepping up! I have never personally used them, but I quit DIYing because I just had a baby and gave all my nic away. But I am curious now as to who the vendors use for nic who I purchase juice from.

 

[carpedebass]

I was thinking that samples would be obtained via anonymous buyer - but yes, that's not as easy as it sounds.

Depending on the scale or nature of any error found, it might be sufficient to first warn the company and give them time to put things right before going public (perhaps issuing a recall if necessary). At some point a name and shame would ensue. I'm not sure the body would necessarily want to get into legal battles, but these could be initiated by the supplier and then the chain issue would arise. So perhaps you are right to an extent at least. It's not such a simple thing to do and might require substantial financial backing.

Indeed! I think you're absolutely correct, that it is a necessity...as is obviously playing out before our very eyes at this moment. In my opinion, to be a responsible user group means we regulate our suppliers ourselves. If such regulation existed to a terrific extent, the "powers that be" involving government regulatory agencies may be less likely to see a true financial reason to deem itself as our regulatory provider.

I am thinking that the genesis of such a chain of custody could begin upon receipt of a sample by a regulatory appointee. However, the appointee (or appointees) should be required to pick up the sample at a storefront type location, as shipping would negate the chain of custody with too many undocumented handlers involved.

All that said, I really think it could and should be done. Of course, what would stand up in a court of law would have to be processed by attorney oversight...that's where things would get expensive in a hurry.

 

[landscaper]

No, not yet. Others have, however, I believe. I'm not exactly sure yet what I would say. I have no demands other than that they test their nic liquids. Don't want a refund. Don't trust them, to be honest. How they handled all this before my tests was really disturbing, and I tend to just avoid people/businesses like that, for better or worse. Might be that needs to change.

I was just curious as to their response because they were so adamant in their previous email about how those test results could not be right.

I'm very skeptical about a lot of these companies, especially those that buy from Chinese manufactures. They don't know what they are getting half the time so how are we to know. We have no idea what someones operation looks like, juice vendors included. Are they making the stuff in their basements or living rooms.

Thanks again Kurt you have done so much to put the warning out and to open a bunch of eyes.

Dave

 

[Kurt]

I was thinking that samples would be obtained via anonymous buyer - but yes, that's not as easy as it sounds.

Depending on the scale or nature of any error found, it might be sufficient to first warn the company and give them time to put things right before going public (perhaps issuing a recall if necessary). At some point a name and shame would ensue. I'm not sure the body would necessarily want to get into legal battles, but these could be initiated by the supplier and then the chain issue would arise. So perhaps you are right to an extent at least. It's not such a simple thing to do and might require substantial financial backing.

I agree, and I am not completely comfortable with the position I am in now. This situation, however, was not first detected by me. People ran indicator tests on BE liquid and got qualitatively similar results and BE was contacted, but the response was very slow, and when it came, it was basically an admonishment that customers would ever doubt the nic levels, and that 200+ mg was impossible. The issue seemed to converge with my own above-described freebase content interests, and so I offered to test samples. Clearly, this is not a case of bad attys or dud cartos. 272 mg nic is beyond dangerous, and supposedly should not even be existing in the public's hands, according to theit mass email, but I am staring nervously at a bottle of it right now, and thus the problem has gone much much deeper.

Only one of the samples I got to test was in the original BE bottle. All others were smaller bottles labeled with the details I requested, so there could be a question of authenticity or validated origin. Regardless, the safety of the community was in peril, previous tests by non-chemists were ignored or ridiculed as erroneous and impossible, the situation escalated to severely dangerous, and rapid communication to the community was, in my opinion, necessary.

Again, its not as though my results came out of left field. They are qualitatively supported by previous tests, while the results of other previously tested nics (MFS) showed spot on accuracy in labeling. It just seems that everyone suddenly takes all this very seriously when a professional chemist does it. This should have been wider news when people used the kits. What does that say about the validity of those kits, regardless of their accuracy?

 

[markfm]

Personally, me only, I would not care to have the final output (as in, say, a bottle of 15mg/ml eliquid) tested every time.

I would care that I, as a DIY type, check my incoming 120 ml bottle of 60 mg/ml liquid, so that I know that yes, it's somehere in the 60 zone. That one 120 ml bottle of nic base, for me, is enough to make a full 480 ml of eliquid, 16 ounces.

The time/$ to do the one incoming check on the 120ml, amortized over the 16 ounces of eliquid I get out of it, is trivial. If I did those checks on each 15 or 30 ml I mix (I actually mix my daily vape 60ml at a time), it would start to become a PITA, and be a noticeable increase in my cost of DIY.

I would likewise care that the artisan eliquid shops do the same kind of incoming check on nic base that I would perform. If I want them to do output checks, on the individual actual bottles of eliquid purchased, great, but expect a cost upper of several dollars per bottle. (the pipettes and cylinders have to be well cleaned to have the rsults come out properly, which starts to take real time if you do many of the checks).

If an individual vendor bought real bulk nic base, a lot, had it sitting around on the shelf, then good practice would be to check it at the time they start using a given bottle.

Going upstream from me, the group that sells me that 60 mg/ml bottle of nic base would, hopefully, be doing the same checks on their incoming product. If they were doing other than rebottling, if they were bulk downmixing, a significant cut from their incoming, then, yes, it would be smart for them to validate their output. My incoming check is only to pick up errors -- they should be testing to make sure there's nothing for me to find.

This is just my thoughts. I usually seek a middle ground. I've been using one nic base supplier all year, without nic testing, and been entirely content with the product. I suspect I'd notice if it was off by more than a handful of mg in the nic base, since I notice the deltas as I'm gradually stepping down the nic in my own eliquids (couple days of increased vaping before I reset to the lower level).

Demanding that titration be done across the board, at all levels, just isn't practical IMO.

If a given vendor does something that specifically skews the results, then that vendor should be absolutely clear about it. For a given vendor doing that it should be feasible to obtain a baseline, wouldn't it? In other words, do the titration series once, on the mg products they sell, and list the equivalent outputs from the BB/acid test?

 

[carpedebass]

I agree, and I am not completely comfortable with the position I am in now. This situation, however, was not first detected by me. People ran indicator tests on BE liquid and got qualitatively similar results and BE was contacted, but the response was very slow, and when it came, it was basically an admonishment that customers would ever doubt the nic levels, and that 200+ mg was impossible. The issue seemed to converge with my own above-described freebase content interests, and so I offered to test samples. Clearly, this is not a case of bad attys or dud cartos. 272 mg nic is beyond dangerous, and supposedly should not even be existing in the public's hands, according to theit mass email, but I am staring nervously at a bottle of it right now, and thus the problem has gone much much deeper.

Only one of the samples I got to test was in the original BE bottle. All others were smaller bottles labeled with the details I requested, so there could be a question of authenticity or validated origin. Regardless, the safety of the community was in peril, previous tests by non-chemists were ignored or ridiculed as erroneous and impossible, the situation escalated to severely dangerous, and rapid communication to the community was, in my opinion, necessary.

Again, its not as though my results came out of left field. They are qualitatively supported by previous tests, while the results of other previously tested nics (MFS) showed spot on accuracy in labeling. It just seems that everyone suddenly takes all this very seriously when a professional chemist does it. This should have been wider news when people used the kits. What does that say about the validity of those kits, regardless of their accuracy?

Kurt, I don't blame you for being uncomfortable. I can only imagine. But allow me to thank you for your analysis and reporting as well.

 

[Kurt]

I was just curious as to their response because they were so adamant in their previous email about how those test results could not be right.

I'm very skeptical about a lot of these companies, especially those that buy from Chinese manufactures. They don't know what they are getting half the time so how are we to know. We have no idea what someones operation looks like, juice vendors included. Are they making the stuff in their basements or living rooms.

Thanks again Kurt you have done so much to put the warning out and to open a bunch of eyes.

Dave

What I am doing takes up maybe 1.5 square feet, other than suddenly having to use a fume hood. It was the 272 mg that really got me angry. Without ventilation, if it was sitting open for a while, you could well start to feel woozy, just from the air. For them to simply deny that this could have happened is beyond concerning, actually creepy to me. I really don't want to go there, it is that scary. I have no wish to get into an argument with that sort. I am very aware, however, that it is very likely my results are going to be a game changer for the industry, especially BE...probably already has. I am admittedly being both carrying for others, as well as very very selfish: people start showing up to the ER with nic poisoning, and my vaping is now under serious threat. I use nic medicinally for controlling nerve pain that is otherwise difficult to treat and remain effective in life. It is far more than just not wanting to smoke to me. It works better than anything else I have tried, and because of vaping I have been able to physically do so much more than I expected I would be able to. In my world, stupid is not allowed to steal that from me.

 

[kinabaloo]

I agree, and I am not completely comfortable with the position I am in now. This situation, however, was not first detected by me. People ran indicator tests on BE liquid and got qualitatively similar results and BE was contacted, but the response was very slow, and when it came, it was basically an admonishment that customers would ever doubt the nic levels, and that 200+ mg was impossible. The issue seemed to converge with my own above-described freebase content interests, and so I offered to test samples. Clearly, this is not a case of bad attys or dud cartos. 272 mg nic is beyond dangerous, and supposedly should not even be existing in the public's hands, according to theit mass email, but I am staring nervously at a bottle of it right now, and thus the problem has gone much much deeper.

Only one of the samples I got to test was in the original BE bottle. All others were smaller bottles labeled with the details I requested, so there could be a question of authenticity or validated origin. Regardless, the safety of the community was in peril, previous tests by non-chemists were ignored or ridiculed as erroneous and impossible, the situation escalated to severely dangerous, and rapid communication to the community was, in my opinion, necessary.

Again, its not as though my results came out of left field. They are qualitatively supported by previous tests, while the results of other previously tested nics (MFS) showed spot on accuracy in labeling. It just seems that everyone suddenly takes all this very seriously when a professional chemist does it. This should have been wider news when people used the kits. What does that say about the validity of those kits, regardless of their accuracy?

Kurt - my point was looking to the future and how a testing body might work and what issues would be involved.

It is in no way a comment on your great work here.

+++

As BE sell 100mg liquid one can reasonably assume that their source is higher than that.

I have seen myself that water and VG do not immediately mix and require agaitation to do so. Probably the same would be the case if the nic was in a PG / water base and added to VG. This might well be the error - not thot=roughly mixing the two, as I think you have already mentioned. It can take more than a quick stir to to achieve a uniform mix and special equipment on timers is often used for this in industry.

 

[Kurt]

markfm, you are right, it is not practical. But it seems more than reasonable when the liquid is potentially dangerous in the first place, such as 100 mg. Possible bad mixing has happened already, and it was openly addressed by the vendor and taken care of (MFS). It can and will happen. Even a simple pH meter probe dipped in a sample will give a pretty good indication of nic content. It needs to be very accurate, but it is totally possible. I would advocate full titration of the dangerous ones, and then use the same pH probe to spot check batches of the more dilute ones. You would need pH readings to 3 places past the decimal, but that's no big deal. Certain flavors would affect this, so it would have to be preflavor liquids. And the affect of the solution not being aqueous would also have to be taken into account, but these things are possible, and once the math is worked out (I have not yet), verification would be quick and easy, or so it seems to me at first thought. Might change my mind on it, but it would certainly point to 2x errors in nic content, which is what we are talking about here, if not more.

 

[kinabaloo]

I was just curious as to their response because they were so adamant in their previous email about how those test results could not be right.

I'm very skeptical about a lot of these companies, especially those that buy from Chinese manufactures. ...

It is likely that the base nic liquid used by BE is the 99% strength, that is then diluted to 10% or less. You can't therefore suggest that the error might be the source as the liquid couldn't possibly be 200% !

The error was in the cutting / mixing. And given the seemingly random values, and that some are over and some under, most likely in the mixing (lack of).

 

[Kurt]

Kurt - my point was looking to the future and how a testing body might work and what issues would be involved.

It is in no way a comment on your great work here.

+++

As BE sell 100mg liquid one can reasonably assume that their source is higher than that.

I have seen myself that water and VG do not immediately mix and require agaitation to do so. Probably the same would be the case if the nic was in a PG / water base and added to VG. This might well be the error - not thot=roughly mixing the two, as I think you have already mentioned. It can take more than a quick stir to to achieve a uniform mix and special equipment on timers is often used for this in industry.

Indeed. But with this its not just mixing physically, its the ventilation too. Open very strong nic is not good. Heating can also make mixing faster and more effective, but that increases volatility of nic to the air. I don't ever want to mix nic.

As for the base they use, that's what I thought too, but their statement was that they ONLY get 100 mg nic, and this is why these results were impossible. So they are either lying, ignorant of what they actually have to mix down, they were sabotaged by a competitor, or there is something far darker going on here. Before we get all x-files on this, I'm going to find the email that was sent out. I think it should be here in front of us again.

 

[Spazmelda]

As I recall, it said something like it is mixed to 100 mg/ml before it comes into their facility, but I remember wondering if it was them who did the mixing, or if they were saying it comes to them as 100 mg/ml.

 

[kinabaloo]

Indeed. But with this its not just mixing physically, its the ventilation too. Open very strong nic is not good. Heating can also make mixing faster and more effective, but that increases volatility of nic to the air. I don't ever want to mix nic.

As for the base they use, that's what I thought too, but their statement was that they ONLY get 100 mg nic, and this is why these results were impossible. So they are either lying, ignorant of what they actually have to mix down, they were sabotaged by a competitor, or there is something far darker going on here. Before we get all x-files on this, I'm going to find the email that was sent out. I think it should be here in front of us again.

Just to be completely clear - i meant BE's error wth mixing (not).

There'd be no profit if there was no dilution; it's hard to believe their source is 100mg.

The handling and cover-up is worse than the crime.

If the error was 'innocent' it's still serious but at least admit it and announce improvements. But even a non-chemist who's selling a product should think of the need to mix carefully and long enough. And final product sample tested.

 

[markfm]

No disagreement, Kurt. I'm actually pro testing, just that at the lower levels in the food chain it should switch from titration to something simpler/cheaper/easier, whether the BB/acid or the electronic probe.

I'm seeing 3 decimal place meters at $500. Undoubtedly someone can find them at a lower price point, though it seems within reasonable reach if someone is a pro, a vendor doing any volume at all. Of course, you then have to keep them calibrated.

For Joe-DIY, small volume like me, the BB/acid would likely make most sense.

Good stuff

 

[kinabaloo]

As I recall, it said something like it is mixed to 100 mg/ml before it comes into their facility, but I remember wondering if it was them who did the mixing, or if they were saying it comes to them as 100 mg/ml.

Hard to be sure. But as 100mg liquid is their main product, I would think it likely that the source is higher concentration. And over ~100mg cannot be sent in parcels, so I would guess thay get it locally.

 

[Sdh]

To all those concerned about recent comments on ECF (E-Cigarette Forum - ECF) about the strength of our Liquid Nicotine products.
Let me try to alleviate any misinformation that may be out there.


The 100 mg/ml strength version of this product contains:
10% L-Nicotine sourced from a reputable supplier in china. (Purity level 99.35%.)
90% USP Grade Propylene Glycol or USP Grade Vegetable Glycerin from a reputable supplier in the USA.
These are rough percentages by volume.

Our formulation methods also take into account the specific compound purities and densities for the naturally occurring stereo isomer of nicotine in its isolated form as well as the specific compound purities and densities for the USP grade Propylene Glycol and/or Vegetable Glycerin.

No other chemicals are added to our product to change the natural aroma and taste of nicotine solutions.

The appearance and odor will be characteristic for this type of product:
Appearance: Colorless, tan, or light yellow.
Odor: No odor, Waxy, or even Fishy.

Recent posts on ECF that were made about someone testing our 100 mg strength VG nicotine at 254 mg strength. While we agree that a simple test kit, such as those available online, may be able to detect the presence of nicotine, such a test will not be accurate in giving the exact milligram strength of nicotine in the tested liquid.

We can assure you that our product is the correct strength of nicotine due to the fact that for safety reasons we dilute our pure nicotine to 100 mg/ml strength before it ever enters our distribution facility. The reason for this is twofold. The first is to ensure the safety of our crew, the second, for the safety of our customers.

Due to the expense of nicotine, any discrepancy in an initial dilution would be recognized as product entered our distribution facility. For example if a dilution were incorrect, we would receive a much smaller amount of our most expensive component.
Due to the large volume that we distribute, and the fact that we do a "50% off" sale about every 45 days, one could conclude that we would not be able to stay in business longer than a few weeks if we were sending out product that was 2.5 times stronger than it was labeled, and at half the price.

With that in mind we would like to announce that for the next week will will be running a "50% Off Sale" on Box Elder Chemical Supply.


Please take note that even 10% (100mg/ml) nicotine is extremely poisonous and poisoning can occur by dermal overexposure as well as ingestion. Users are recommended to do their own research on safety precautions and follow label instructions when handling this product. Good information about this subject can be found on ECF. (E-Cigarette Forum - ECF).


Sincerely,

Brad Bacher
Box Elder Chemical Supply
888-962-5877



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[kinabaloo]

No disagreement, Kurt. I'm actually pro testing, just that at the lower levels in the food chain it should switch from titration to something simpler/cheaper/easier, whether the BB/acid or the electronic probe.

I'm seeing 3 decimal place meters at $500. Undoubtedly someone can find them at a lower price point, though it seems within reasonable reach if someone is a pro, a vendor doing any volume at all. Of course, you then have to keep them calibrated.

For Joe-DIY, small volume like me, the BB/acid would likely make most sense.

Good stuff

Like this ?

http://www.e-cigarette-forum.com/fo...st-mg-ml-nicotine-follow-up-dvaps-method.html

This assumes I think that the e-liquid has not been acidified (already), but otherwise is simple, once one has the two required chemicals.