final product separation at the market

Dear all,
I would really apreciate it if you could express your opinion. In the small production unit that I work, we have bought a new high sheer mixer(unfortunately not a silverson or something with regards). I tested it and seemed to work fine, so I passed in the production scale in liquid matte lipstick. Its a product that I have been producting for one year now with a lab homogenizer with upscaling capacity, with stability test,and none a complain from our clients since now.
after the microbiological test of the batch, I released it on the market in stores. 3  days later, a lot of returns anc complains started. 
it seems that an oily colorless layer of some ingredient, is coming out of the packaging and dries out like a sticky glue. My guess is isododecane, or maybe some of the silsesquioxane or an other silicon of the formula.
Is it possible in a stabilized product, a change in the production equipment to bring such a disaster?
and an other question for whom has been worked with liquid matte, do you think that the fillling machine must be under medium heating(e.g 40 oC) and stiring, OR that 'maltreats' the product?
Thank you in advance for any thoughts or advice

Comments

  • edited August 2018
    Let me know if you'd like some assistance in your investigation.  I work with one of the largest scientific and engineering consulting firms in the US.  We do a significant amount of R&D and failure analysis support.  Feel free to message me directly.  
  • PerryPerry Administrator, Professional Chemist
    Yes, it is possible that a change in production procedure can cause a stability problem. Especially, if your manufacturing change is the type of mixer you are using.  And especially if you are going from lab sized batches to production scale sized batches!

    Without seeing the formula or ingredient list, no one will be able to guess what is the problem. I'm thinking you didn't create a good enough emulsion in the production process.

  • I would expand on what @Perry said by adding that it would be helpful to analyze the oily layer, perhaps by FTIR or a chromatography technique, and compare it to your raw materials.
  • edited August 2018
    @marytsiang you may need some heat? can you write down the ingredients list?
    Dr. Catherine Pratt
    (B.Sc with HONS I , Ph.D Analytical/Organic Chem and Microbiology), Cosmetic Chemistry IPCS)
  •  

    ISODODECANE

    25% 

    HYDROGENATED POLYCYCLOPENTADIENE

    5% 

     

    DISTEARDIMONIUM  HECTORITE

    5%

     

    POLYETHYLENE

    5%

     


     

    POLYMETHYLSILSESQUIOXANE

    5%

     

    HYDROGENATED TETRADECENYL/METHYLPENTADECENE

    5%

     

    PROPYLENE CARBONATE

    1% 


    COPERNICIA CERIFERA CERA

    1%

     

    TRIMETHYLSILOXYSILICATE

    1%

     

    ALUMINA

    0.1%

     

     ALUMINUM HYDROXIDE

    0.1%

     

    TRIETHOXYCAPRYLYLSILANE

    1%

     


     

    PROPYLPARABEN

    ≤0.1%

     



     B.H.T.

    Dear all, here is my ingredients list. I would really appreciate it, if could share your thoughts.


    ≤0.1%

     

  • @Perry @DrCatherinePratt @DrAndrewWorthen I heat it up to 80 degrees celcius. Im not sure about how to create a stronger emulsion.Do you think from the ingredients list that there is a stability problem?
    An analyze of the oily phase would be a great option,to see what ingredient did not homogenized to the others.. 
  • @marytsiang  there is a totally different problem it could be. Have you thought about the formula reacting with the new machinery as you have Alumina in there? What was your homogeniser made out of previously? Also can you put in some more BHT? Or Tochepherol@ 1%. 

    Dr. Catherine Pratt
    (B.Sc with HONS I , Ph.D Analytical/Organic Chem and Microbiology), Cosmetic Chemistry IPCS)
  • Similar situation happened to be, but in our case, we identified the issue in the pilot run rather than full production.
    What helped me to figure out the problem was doing a root cause analysis. 
    The root cause in my case was the emulsion instability. It was separating but we didn't catch in the lab tests prior pilot tests for a simple silly reason: In the lab tests (stability tests) the cans were shaken before sprayed, so the emulsion was back to one phase, while in the compatibility tests (after pilot run) the samples were not shaken before sprayed.
    So, the root cause analyses pointed this out and we were able to confirm it.
    I would try the same thing.

  • makamaka Member
    edited October 2018
    Are you sure that the formula was stable? Have you done any F/T testing? I've experienced a lot of problems when gelling Isododecane..liquid was separating from the bulk etc.
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