E-liquid Chemical Analysis

Discussion in 'The Vape Merchant' started by Mauritz, 17/5/17.

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  1. Mauritz

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    Hi Vape Geeks,

    In the coming days we will start publishing certificate of analysis for some products we are manufacturing for our clients. I wanted to take a moment to discuss how we are doing chemical analysis and what we are testing for.

    We use the Rancimat machine to establish a best before date. The Rancimat determines the oxidation stability of natural fats and oils, in their pure form as well as in fat-containing foods, cosmetics and pharmaceuticals . It accelerates the aging process of the sample by exposing it to heat and increased volumes of air, and it measures the time that passes until oxidation takes place. This then gives us an index by which we can establish the best before date.


    We also use a method called gas chromatography - mass spectroscopy (GC-MS). The headspace injection technique is used to detect low levels of volatile components in liquids. Volatile sample components defuse into the gas phase at 150 degrees c and this collects in the headspace. This is the ideal technique to detect residual solvents, chemicals in flavourants, alcohol and nicotine levels.

    The output looks something like this :

    [​IMG]

    This gives us a unique finger print of all chemicals present in the liquid. We are specifically interested in the below chemicals but keep full record of all compounds should we need to refer back later.

    We measure these in parts per billion.
    • ACETOIN ug/ml
    • ACETOL ug/ml
    • ACETALDEHYDYE ug/ml
    • ACETYL PROPIONYL ug/ml
    • ACROLEIN ug/ml
    • DIACETYL ug/ml
    • DIETHYLENE GLYCOL ug/ml
    • 1,3 DIOXANE,2 METHYL ug/ml
    • FORMALDEHYDE ug/ml
    • ISOPRENE ug/ml
    • n-NITROSONICOTINE ug/ml
    • TOLUENE ug/ml
    • COTININE ug/ml

    Lastly we test for bacteria, yeast and mold using the micro method. Once completed we generate a certificate of analysis.

    And there you have it folks. A brief overview of how we ensure that your favorite e-liquid is safe and that you are vaping pure excellence.

    Open to any questions for those with a curious mind.

    Regards
     
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    Last edited: 18/5/17
  2. Andre

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    Interesting, what is your average period for best before date? Does it differ according to nic content, category of juice, container, etc?
     
  3. Mauritz

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    Hi @Andre,

    Great question !

    In short, we still working with limited data. All batches tested to date are stable for at least 12 months. The batches tested so far represent a full spectrum from a nicotine and flavourant perspective. Our approach is to archive these samples for one year and retest 12 months later. Should the product still show viability we will issue a notice to the particular vendor. They can in turn then update their clientele.

    As we gain more data we plan to publish research papers on the topic to establish a solid scientific base for the industry to grow on. We are also conducting research on the impact and toxicity of long term exposure of various chemicals with the aim to publish our findings as well.

    Some factors to consider :

    1. All batches tested have been manufactured in our lab. We adhere to strict quality control processes which eliminates contamination from bacteria, yeast and mold. If a product is manufactured outside of these conditions and/or contamination occurs it will reduce the lifespan.
    2. The Headspace technique exposes the product to 150C for 48 hours. Temperatures exceeding this threshold or timespan will reduce the lifespan.
    3. UV light ( from sun or other sources ) will reduce the lifespan. From this we can conclude that amber or otherwise opaque bottles will result in a longer lifespan.
    4. Generally speaking glass best. However HDPE plastics are chemically stable and should not leach into the product unless exposed to UV light. PET is generally regarded as safe but will break down and leach much sooner than HDPE. The concern here is exposure to the leached chemicals rather than accelerated breakdown of the e-liquid.
    5. Products with a higher PG to VG ratio will generally last longer as the PG displays antimicrobial properties. In addition, Acrolein is a byproduct of VG manufacture and higher concentrations of VG will lead to higher concentrations in the final product.

    Please let me know if you have any further questions.

    Regards
     
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    Last edited: 18/5/17
  4. RichJB

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    Fascinating stuff, thanks for sharing @Mauritz. Will you be doing any testing of DIY flavourings? I am always concerned that my flavours will degrade if I don't use them up quickly enough. There seems to be very little info available on this, with some DIYers reporting that their concentrates degraded, changed colour and lost potency after a period, others saying their concentrates have lasted for years without any noticeable change. It would be handy if the industry could establish some sort of lifespan benchmarks for these concentrates.
     
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  5. Mauritz

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    Hi @RichJB ,

    We will indeed. This is crucial for us from an ISO 9001 perspective as we need hard facts on the viability of our input ingredients. This may take some time to conclude and will vary wildly from flavour to flavour. Will absolutely post our findings here.

    We have already identified some high Dioxane levels in some flavours. We are waiting on feedback from those flavour vendors before we report our findings. Dioxane is found as a residual solvent in PG. While there is no established safety limit for it, it would be best to keep Dioxane levels as low as possible as it is a know human carcinogenic. That said, the maximum level we detected was 34.7 parts per billion. This is a very small number and estimated exposure levels are considered to be lower than those that might constitute a danger to human health. This is echoed in this article if you want to know more

    http://davidsuzuki.org/issues/healt...etics---peg-compounds-and-their-contaminants/

    Isn't science fun ;)

    Let me know if you have any more questions.

    Regards,
     
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  6. Max

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    In other words @Mauritz - GC - Gas Chromatography & Oxidation Stability - I sincerely appreciate the accuracy of this Process.

    My Business is totally based on DG Analysis - the data capture of that information on a specific database and the Trend Analysis there of.

    Looking forward to feedback on your associated case studies.
     
  7. Mauritz

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    Hi @Max ,

    Appreciate the response. We really are focused on creating better products through good science.

    Regards
     
  8. Max

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    Hi @Mauritz ,

    If there's a Thread on this Forum - it's going to be this one.

    Knowing the accuracy of Headspace GC Analysis - and it's cost per Vial - You have all my respect doing these tests.

    Thank You so much for all your efforts
    to obtain this important information.

    Best Regards
     
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  9. Silver

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    This is fascinating
    Congrats on it @Mauritz
    Am watching with great interest
     
  10. Cespian

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    Beautiful thread. Subscribing.
     
  11. Mauritz

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    Hi All,

    Another week, another finding.

    We decided to raise the temperature on the GS-MS process to see what happens. We usually test between 120-150 C but this week we decided to take up the heat to 200C and found propanamide 2 hydroxy also known as Lactimide at concentrations of 441 parts per billion. This seems to be a result of the VG reacting Nitrogen dioxide in the flavourants.

    Now, don't be alarmed. Lactimide is not classified as toxic or carcinogenic. I have linked to study below for those die-hard scientists. In short, studies have concluded that while no inhalation risk data is available, oral and dermal single and repeated exposure lacked systematic toxicity. Also, negative results for genotoxicity in Ames tests and an unscheduled DNA synthesis assay, and little to no irritation potential and no sensitization potential.

    http://www.cir-safety.org/sites/default/files/amides032012FAR.pdf

    Also to consider is that the concentrations are low and total daily exposure would be very limited.

    Hope you find the information interesting.

    Regards,
     
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  12. RichJB

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    Let's keep this to ourselves, @Mauritz. I don't want to be told by ou tannies that my Twisp is going to give me Lactimide Liver. :p