Pit Vaper

Copied from that other forum but important none the less...

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

Just to bring people back up to speed with this issue, several people here suspected that their Box Elder unflavored nic was too high compared to the labeled concentration. Someone claimed to have tested that theirs was 240 mg/mL. Others stated that theirs was also strangely strong. I, on the other hand, suspected mine was just different somehow, since it had no TH and very little odor in the 100 mg VG I bought. I offered to run full titration pH-curve analysis on any nic that was sent to me, since I was interested in nic level as well as freebase/nic-salt ratio. Several sent me samples of theirs, and I am presenting the results here, after spending much of the day doing these as accurately as possible.

At some point during the discussions, BE decided to send an email out to all its customers stating that it was impossible for anyone to receive >200 mg nic, and people should be assured that whatever the nic level was that was ordered, that was the nic level received.

Titration curves are not difficult to obtain, but to do them accurately requires specialized glassware and electronics. In my 30 year career I have done 1000s of such titrations.

What I did: I used a PASCO pH probe calibrated to within 0.001 pH points at buffer pHs of 4, 7, and 10. I also used a calibrated PASCO drop counter, allowing accuracy to within about 1/30th of a mL during the titration. I used volumetric pipets and volumetric flasks to make dilutions for the nic liquids to be titrated, and I titrated with standardized 0.0730M HCl. pH at 0 mL titrant was measured to estimate freebase/salt ratio, and pH curve was created to past the first equivalence point (2nd inflection point). Each nic sample sent to me was titrated 3 times at least, and most samples sent were enough to do another set of 3 titrations. The nic concentration was then calculated from the titrant volume at the first equivalence point, back calculating to the original sample concentration.

All samples, including my own sample, were virtually all freebase form, base on initial pH and final nic content found.

I will give the results in two columns. The first is the nic content as given on the label. Second column will be the nic conc as determined by the above method.

Nic labeled.....Nic determined

100 mg....48 mg (This one was mine. Thanks BE.)
100 mg....120 mg
100 mg....272 mg
48 mg....78 mg
36 mg....51 mg
48 mg....59 mg
100 mg....98 mg (this was my MFS 100 mg VG)

I would say the intrinsic error is less than 2% for all of these. These results are as accurate as is obtainable, IMHO. I knew the one that gave the result of 272 mg was way high when I opened it, as it was so strong in nic odor that I had to work with it in a fume hood for the dilutions. It was also honey-amber, whereas the others were either colorless or slight yellow.

272 mg nic was likely the base they diluted to 100 mg from, or else they were mistakenly sent a lot of 100 mg nic that was actually 272 mg.

I don't give a rat's a$$ what their excuse is, someone could well have died from this! I am a seasoned chemist, and this liquid was seriously scary to work with. Clearly there is more concern with CYA than actually testing their nic. Had they been responsible and expressed concern and actually tested their nic, this might have been avoided, but they instead chose to lie and even condescend as to how ridiculous the idea of levels being sold wrong was, and how oh so professional they are.

For this community, this is about as bad as it can get. I strongly recommend Box Elder be banned from ECF, and the word should be spread to other ecig forums. The FDA would have a field day with this. If others want their nic analyzed, PM me.

Vendors, you are now on notice. Either self-regulate and KNOW what you are selling, quantitatively, or else you are putting people, as well as the industry itself, in grave danger. I have no problem buying small quantities of unflavored nic solely for testing purposes. You have been warned.

I am seriously outraged by this.

Kurt
Quantum Vapyre ECF Veteran

mrwizard

I was following the original thread until it was closed.
At the time, the only complaints were regarding BE VG bases.
This could've easily been due to the thick viscosity of VG and incomplete mixing of the primary batch leaving "hot spots" that were then put into smaller bottles.
Many people assumed that if they had a bottle of PG base they were safe, however, in this latest thread, Kurt posted that his high readings came from PG bases.
This means that ANY bottle of BE you have could be mislabeled or incorrectly diluted.
This is the kind of thing that will shut vaping down.

berger

Is it just box elder though?..who was the original supplier of nic to them...they stated they were only getting 100mg/ml nic from their supplier...is this a bigger problem or solely a box elder issue?

mrwizard

It was my understanding that BE buys pure nic, and dilutes it down to 100mg/ml as a first step.
Then uses the 100mg/ml to mix down to the proper level for the final product.
Either way, quality control rests squarely on the shoulders of the company doing the final consumer packaging.

This could've been avoided in a couple of ways.
Simple record keeping would've shown the amount of first stage product did not equal the correct sum of the beginning ingredients.
A basic 5-minute test of the first stage batch, or nic supply from the mfg. would have shown an obvious variance.

This kind of negligence will shut down the vaping industry quicker than any other political threat.
Public safety trumps all, and there is no room for error.
The Wild West days of vaping and vending are coming to a close.

mrwizard

Since BE supplies nic base to other vendors as a wholesaler, this problem could be widespread.
How widespread, who knows?

Rocketman

BE also supplies other vendors.

Where is the recall?

What lots codes and what concentrations, are suspect?
(your nic does have a lot code, right?)

Is this being investigated, like officially?

Have unopened, sealed samples from BE been tested?

Which vendors that dealt with BE are now suspect?

Have you contacted YOUR vendor for any unflavored nic in your freezer?

berger

Yea..this could be a huge problem..too bad Pbusardos nicostrips joke never actually came to market
is something like that even feasible?.. I know there are the test kits...hmm...almost to market from a trusted supplier round here...nudge nudge...(put me on that list)
but lets face it..unless there was an easier way most people aren't going to bother. Im not saying the responsibility for this should fall to the consumer but the reason many arent testing is cost and time...something simple like that could go a long way to discovering and or avoiding this for everybody..Is it even remotely possible?

mrwizard

None that I'm aware of on both counts.
I think someone will have to file a lawsuit before we'll see any form of investigation.
I'm surprised that hasn't already happened in our sue-happy society.
That's the million dollar question.
Looking at some of the other posts mentioning mislabeled product #'s in addition to mislabeled product contents... who knows?
Yes, as well as the PG and VG.
The only labels that didn't have a lot # were the original test samples/labels that I sent around months ago.

That's a very good question.
I imagine if there were enough demand and research funds available, a test strip could be developed, but I'm not going to hold my breath.
It's only recently that test strips were finally developed for more than basic pH testing in the aquarium trade, and that's a huge market compared to vaping.

The simple titration test developed by DVap is accurate, cheap, and easy enough for our purposes... and yes, I'll be making it available along with a more accurate, scaled-up version.
Sorry for the delay, big guy, but that opening day fiasco exposed a lot of areas that need to be corrected and streamlined.
I'd rather take my time and do it right than rush the process and risk a mistake.
Right now I'm selling off my old aquaculture stuff to make room, and free up some more funds.

berger

Understood Mr Wizard...just a friendly prodding..I'll be waiting patiently..sort of...

RY4

Wow. Wow. Yeah, this kind of stuff just makes me want to get over my fears of mixing and handling nicotine and just jump right in. From a consumer stand point, yes, I can see needing to test and make sure you have received the level you purchased but come on..... how many consumers test everything they buy to make sure it is indeed what they bought. We don't go around testing milk, sodas, shampoos, prescription drugs, vitamins, etc... we assume it is safe with the regulations in place until something happens then the gov steps in with its safety measures. As much as I hate to admit, there does need to be regulation of some kind with this issue arising. Public safety does trump all and it really ticks me off that the supplier didn't take the time to be responsible to ensure the safety of the product.

mrwizard

LOL
At least you don't have to wait patiently for one thing anymore.
PM'd your tracking #.

You're absolutely right, on all counts.
Yeah, regulation is going to mean a little higher prices in the end, but what price can you put on a human life?
I've said from the beginning we need some form of regulation.
Self-regulation has never worked successfully in any industry before.
How stupid is it to have a completely unregulated industry who's main product for human consumption could kill an adult with a single drop?

wetwire

Thought it was two ..

The real shame is that, its the same old thing about the one bad apple. I would guess that many other vendors pay careful attention to detail and care enough about their customers to do things as safely as possible. All this over one wormy apple.. so far.. that we know about. Makes one wonder how many down the line were affected by making an end user product. How would they know. Considering testing seems to be a fairly recent concept for most.

LeCig

This is exactly why we'll never sell more than 36mg ... and as for DIY, well, I'd rather stay away from that too.

The TVECA is a trade organization that we belong to. Our goal is to set standards in the industry that will stop anything like this from happening. I believe in consumer choices, but when it comes to mixing imo it needs to be left up to the pros. If a noob did get 1000mg nic and try to cut it I can see room for error.

The regulations are coming ... tic toc.

mrwizard

That's probably the smartest choice, Mike.
Unfortunately so long as there's a demand, there will always be someone supplying.
The best we can hope for is good regulation to help keep the worst offenders out of the market.

Good on ya for belonging to a trade organization with a responsible goal.
*thumbs up*

LeCig

Thanks!

You can find out more about the association at http://www.tveca.com/

mrwizard

Actually depends on the size of the drop.
A standard dropper bottle cap dispenses ~20 drops per milliliter.
1ml of pure nic = 1000mg
1000mg / 20 drops = 50mg per drop
Estimated fatal dose for an adult is ~50mg and for a child is ~10mg according to most of the papers I've read, so 1 drop of pure nic can be fatal.

To the best of my knowledge, until DVap developed and published his original expanded and simplified titration methods at the end of 2009, there was no one doing any testing of any kind. How many vendors actually read his post and put it to use afterwards is anybody's guess.

Professional lab testing is far out of financial reach for any small vendor, and I seriously doubt that any of the large vendors are sending off samples of each batch for testing either.
When I first started looking into mixing nicotine base, I shopped around several labs for an independent analysis to compare against the manufacturers' analysis.
The cheapest quote I got was over $1,200 for a partial USP.

Although it can't test what other impurities may be present, at least with DVap's titration test we're able to compare stated nicotine content versus actual content, and in my opinion that's the primary risk to the consumer.

On a sidenote, I've always been a bit concerned over how thoroughly a pure VG base mixes with nicotine. It's been mentioned several times before, but if you are buying 100% VG nicjuice you really do need to work under the assumption that it has not been completely mixed. There could very easily be "hot spots" or layers of pure to near pure nicotine in the bottle.
The BE situation just highlighted it for me.
When I first heard about the problem and it was only reported on VG bases it definitely made me wonder about any pure VG nic bases I've mixed or shared.
I've even been considering not offering 100% VG that hasn't been cut with at least 5-15% water to make sure it mixes completely.

I set-up a quick visual example to make the point. Now, this is not meant to be a true scientific test of actual mixing procedures or packaging. No one is mixing nic in tall, narrow containers like test tubes (at least I hope not!), but it does make the problem easier to see.



The first photo is a couple of drops of food coloring in a test tube of 100% VG.
The second photo is the same test tube after 90 full seconds of constant inverting and vigorous agitation... or as Rocky would say... shaking the "sheet" out of it.
We can all see the huge difference in concentration between the top of the test tube and the bottom.
This could also happen in a normal container that's been filled to the top to eliminate any headspace before mixing.

The third photo has the original test tube for reference on the left, and on the right is a test tube with a couple of drops of food coloring and a mixture of 80% VG cut with 20% water. This makes the VG approximately the same viscosity as PG, which Rocky confirmed in his previous viscosity tests which I can't find right now or I would post a link.
The fourth photo shows that even in a tall, narrow test tube, when reduced to the viscosity of PG, a "pure" VG nicbase will mix completely even after only 10 seconds of shaking.

On a side-sidenote, I filled a typical 60ml bottle commonly used for unflavored nicjuice with pure, undiluted VG and 1ml of food coloring.
I did not overfill the container and left about a half an inch of headspace.
I shook it for about 15 seconds and poured the contents out into a beaker.
The food coloring did mix pretty thoroughly, but I would still advise mixing well any unflavored VG nic bases you may have ordered, and if it's from BE, don't use it until you run a nic test or have someone like me or Rocky run a test on it for you.

mrwizard

Thanks for the link.
Checking it out now.

berger

So what your showing is...your tube needs more head?....

mrwizard

Who's doesn't?



17 posts until we're reminded this is Vapeatron.
Geez, that's gotta be some kind of record!

CountryCarolyn

I know you aren't going to believe this but I can taste when water is mixed in the vg.

mrwizard

When it comes to our Betty Crocker, I believe anything.

Hi CC! Glad to see you're back... on both forums. I'd hate to lose you again. I don't even have your email addy.

CountryCarolyn

Well I missed you Mr Wiz and of course Rocket!! Well I will have to get you my email, cause who knows about me. I may go spouting off at any moment, hee hee!!

You can always find me on facebook, and on twitter now. Elixir, outcastvaping, or even vapetv. You know me I can't sit still for to long.

Facebook is just simply Carolyn Carter. Twitter is CountryCarolyn_ everywhere else is CountryCarolyn.

You know I tested some juice I won that was from pink spot vapors. You know it tasted like it had water in it. I drink probably close to a gallon of water a day. That is one taste that I am very keen on.

LeCig

You using distilled?

CountryCarolyn

@Mike I don't dilute my vg. I have just had juice that has been diluted.

@Pit I know you are like me and watch the stickam shows. Well I just wanted to let you know that Brad from box elder is going to be on vapetv tonight with Cozziecon @ 10 pm!! I am assuming that is est.

wetwire

Well this could be a total mistake but, as I have stated before. I nuke my mixes before use to make blending everything together much easier and quicker. So far I have not found any adverse reaction to this method. I only nuke them for 6 seconds at approx. 10-30mls at a time and it is used fairly quick. Some of them have set for a couple of weeks, not being completely used yet. When I have gone back to use them, they seem fine. The reason I bring this up is, I wonder if it would be a suitable practice for thoroughly mixing the base nic. Also, is there anything that suggests that the nic could separate after it has initially been mixed in PG or VG. Can it settle is what I am trying to say. I think the answer would have to be yes, but the real question would be. How long does this process take. A year? Five?