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

  1. #1
    Quantum Vapyre ECF Veteran
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    Default 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....121 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)

    * edit for above added at end adding vehicles and BE lot numbers and purchase dates, if known


    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 ..... 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.

    **
    edit to add :

    So to give the list again now with vehicles and BE lot numbers and purchase dates, if known:

    100 mg....48 mg (This one was mine, don't know lot #) VG 6/9/11
    100 mg....121 mg PG lot 256 7/5/11
    100 mg....272 mg VG lot 257 5/29/11
    48 mg....78 mg VG lot 257 9/7/11
    36 mg....51 mg VG lot 257 8/27/11
    48 mg....59 mg VG lot 257 6/11/11
    100 mg....98 mg (this was my MFS 100 mg VG) 1/1/10
    Last edited by classwife; 11-19-2011 at 08:22 PM. Reason: added final date
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    OMG!!! Are you serious?!?!?! That's bad, real bad. Someone could be seriously injured from this!

    I agree, they should be banned for not taking this issue seriously. Someone somewhere screwed up, and we'll all pay if it's not controlled better by our vendors. They should have been testing everything as it came in and not making assumptions.

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    Ultra Member ECF Veteran Lyndagayle's Avatar
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    This absolutely blows me out of the water!!! I totally agree with the ban and spreading the word. Thank God we didn't have a tragedy result from their poison. I wonder how many vendors have been using their product???? This stuff could be all over the place!
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    I can't believe that box elder is completely not addressing this issue. Obviously there is the ethical issue with the safety of your customer. Not to mention the financial issue that Box Elder will face and the political issue we could all face if and when someone gets seriously ill or worse and then sues.

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    Holy Frickin Cow!

    Those data are horrible. I have been holding off with my next nicotine purchase until I saw your data, Kurt. I will do my part and vote with my wallet. Going back to Xtreme with my next order as a little bit more $ seems all the more worth it.

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    smallmam tested RTS liquids and they came up fine with her method. She used br-blue indicator and H2SO4. From her posts in the original "BE too strong" thread:

    "#1 16mg box elder 100mg VG 30ml
    4.6ml-3=1.6
    1.6*19.4712=31.15392mg

    #2 16mg box elder 100mg VG 3ml
    4.7ml-3=1.7
    1.7*19.4712=33.10104mg

    #3 16mg RTS 100mg VG 3ml
    3.7ml-3=0.7
    0.7*19.4712=13.62984mg


    #4 16mg box elder 100mg PG 3ml
    3.8ml-3=0.8
    0.8*19.4712=15.57696mg

    #5 16mg RTS 100mg VG 3ml
    3.8ml-3=0.8
    0.8*19.4712=15.57696mg

    #6 16mg box elder 100mg VG 3ml
    5.0ml-3=2.0
    2.0*19.4712=38.9424mg

    #7 16mg box elder 100mg PG 3ml
    3.8ml-3=0.8
    0.8*19.4712=15.57696mg

    #8 16mg box elder 100mg VG 30ml
    5.0ml-3=2.0
    2.0*19.4712=38.9424mg

    I have made 3ml liquid of box elder VG 100mg, RTS VG 100mg, box elder PG 100mg. 0.48ml each of nic with 2.52ml of PG to make 16mg liquid. I do use separate syringe for nic and PG and VG and water.
    I diluted with PG only except 30ml ones. 30ml ones contain PGA. none of them is added flavorings. I have shook all the bottle before I inject into syringe. injected needle to center of liquid.
    I have cleaned 10mL Graduated Cylinder 3 times with Distilled Water between each test.I have run these test 8 times I do believe I am getting hang of it. but if you are curious about this, I'd send sample of this box elder VG 100mg nic to you with your own risk."

    So I think she is doing fine within the accuracy of the method itself. Again, BE is too high by about 2x. But 272 mg?? When it was stated that this is "impossible"?? That's the part that makes me really angry.
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    Have you tried to contact them about these results Kurt? I'm curious as to what they would say (or not say since it took them over a month to address the original issue in the first place).
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    Although I don't DIY I am very thankful there are people like you that take the time to keep us all safe. Your work will make everyone's vaping experience safer.

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    So I can assume my 36ml Box elder pg nicotine is not up to par. Gourmet vapor utilizes Box elder's nicotine. Very scary indeed. I have used very little of this Box elder. Thank you for your testing.
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    Thanks for posting Kurt - good job! You are an angel to do this for us. Gratitude and love to you.

    I have copied your entire results to my hard drive in case your post ever myteriously disappears.
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