Problem with shampoo

I have noticed a problem while preparing a shampoo. When all the ingredients (w/o api) are added, the shampoo is let to defoam for about 24hr. After the shampoo is clear, a crust on the top of the shampoo is formed. It has some kind of gel consistency.
Anyone had this problem?


  • You forgot the list of ingredients.
    What is w/o api?
  • edited September 2017
    Sorry, you are right. Below are the ingredient used. w/o means without api. The api is added as the final step.

    Sodium Laureth Sulfate, Cocamidopropyl Betaine, Disodium Laureth Sulfosuccinate, Hydroxyethylcellulose, Butylated Hydroxyanisole, TEA, NaCl

  • Is the shampoo storage container sealed, or left open to the air?
    Robert Zonis, Sr. Formulation Chemist, Beaumont Products "All opinions and comments expressed are my own, have no relation to Beaumont Products, are fully copyrighted, and may not be used without written permission."
  • sounds like surface drying which can happen even with a sealed container with big head space.
  • edited September 2017
    This didn't happen too often when I was formulating shampoos but we used to just skim off the top layer when it did. It was usually just dried out foam. I think adding a humectant like glycerin might help.
  • The shampoo stays in the container of the machine where it is homogenized, which has a big lid.
    @Perry, yes, but the loss is around 5-10% which I think it is too much. How much glycerin would you suggest to add? 
    Any other idea? Would it help to put the shampoo to an other container(s)? 
  • That's a lot of loss. 

    You didn't list Water in your formula. Is it in there?  If not, diluting it should help reduce the foam and loss.
  • It has a lot of water, I will come tomorrow with the percentage of the water if needed. Adding more water will indeed reduce the foam but the product itself when used to wash doesn't foam that much like in commercial shampoos. 
  • A 10% is too much, I'd think your product didn't homogenize, seems more like phase separation. It is a cold process or do you heat up the components?. Even if theoretically the components would blend @RT, sometimes they don't. It happend to me with a similar formula, but I was using DEA. 

    You should take some right after blending in a test tube and see how it behaves. 
  • It is a hot process. I was thinking the same. 
    Next time I will take a sample and put it in a small container and seal it to see if it behaves the same as the rest of the product.

    Thank you for the help everybody! 
  • So water is around 55%. First thought was, SLES was in high concentration, but reducing it, did not improve anything. I'm going to add each separately one by one and see when and what happens after each ingredient. 
  • I was wondering, where and how do you homogenize?. Given the thixotropy of the shampoo I guess you are mixing at 40-60 RPM. Depending on the configuration of your homogenizer and the paddle setup you must consider specific weight as a potential problem. 

  • It is homogenized with standard homogenizers used for semisolids and shampoos. The mixing speed is indeed 60 RPM (if I'm not wrong, will confirm it shortly). The formulation is made with two different homogenizers (smaller and bigger), but the result is basically the same. What is the average time to let the shampoo in repose state? Will it be better if the time is longer, lets say a few days, or a week?
  • Why are you using BHA in shampoo? I found this:
     The European Union prohibits the use of BHA as fragrance ingredient in cosmetics. The State of California requires warning labels on products containing BHA, notifying consumers that this ingredient may cause cancer.
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • @em88 what's your method of manufacture? HEC has to be hydrated correctly or else it'll separate from the rest of the batch

    @Belassi on the contrary, BHA is not subject to any legal restrictions in the EU, nor has IFRA restricted its use in fragrances

    my only comment is that in this particular instance it's unnecessary - there are no oils prone to oxidation in the formula
    UK based formulation chemist. Strongest subjects: hair styling, hair bleaches, hair dyes (oxidative and non-oxidative) I know some stuff about: EU regulations, emulsions (O/W and W/O), toothpaste, mouthwash, shampoos, other toiletries
  • @Belassi It is used as antioxidant, it will increase the stability of the API ;) 
    Bill_Toge, HEC is the first ingredients which is used to make the gel and than the rest of ingredients is homogenized in it (using temperature 60-70 C)
    I first suspected about HEC to be separated, but the quantity used is less than 0.4% while the crust formed is between 5-10%. 
  • Your problem is most likely due to air and foam:in addition cellulosics like HEC form a film at the foam /air interface making the problem more difficult.Try making a stock solution of HEC and adding sub-surface during cool down.
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