Bubbles in formula

Hi,
I am trying to come up with a formulation for a shampoo. But the problem I am having is making the Xanthan solution. The formulation includes- Glycerin
Xanthum Gum
Monopropylene Glycol
Aqua
Decyle Glucoside
Cocamidopropyl Betaine
Cocamide DEA
Dimethicone
Benzalkonium Chloride
The way I am trying to mix the Xanthan (0.5%) is by first dispersing it in glycerine and then adding it to water which has been heated to 70 degrees and then mixing it extensively. After mixing small bubbles form which do not go away. Any help would be greatly appreciated.

Comments

  • BobzchemistBobzchemist Member, PCF student
    What's the typical size of your production batch?
    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."
  • BarrowBarrow Member
    edited July 2015
    Thank you Mr Bobzchemist. I am sorry I should have included more details. The Xanthan (0.5%) is dispersed in Glycerine (5%) and then added to water which is about 66%. It has been only 50g batches so far. I have been doing it in weights rather than volume as it is easier to measure. So will changing the respective percentages affect the small bubbles or is it a mixing error? Last time I used a mixer to do it. Thank You
  • AylaAyla Member

    Try dispersing the xanthan in monopropylen glycol instead of glycerin. Then add it in water and mix slowly. No bubbles !

  • BobzchemistBobzchemist Member, PCF student
    Sorry, I didn't realize you were just a hobbyist. But even for a hobbyist, 50g is way too tiny to be representational of anything your going to get when you make a batch large enough to actually shampoo hair with - it's barely a thimble-full.

    In simple terms, you should ignore almost everything that happens in a 50g batch. It's like building a toy car with toothpicks and thinking that any information/results from doing that will translate into what would happen if you built a full size car.

    If you start making a more realistically sized batch, which is usually a kilogram, and you still have bubbles, buy a vacuum pump and a vacuum flask (with a stopper). Several minutes under vacuum will pull out bubbles from almost anything.
    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."
  • MicroformulationMicroformulation Member, Professional Chemist
    Agree with Bob. Also, in a shampoo 5% Glycerin could have an effect on foaming and foam height.

    Even in my lab with prototyping I make 0.86 KG batches. (Weird number but it is 12 ounces plus a small loss factor which is enough to support testing as well).

    Mixing surfactants is definitely an area where you have to take care to mix slowly. You would really need a variable speed blender to do this, which I hope you have. A stick blender is a recipe for disaster in these products.
    markfuller@microformulation.com Microformulation.com Microformulation Cosmetic Consulting provides Custom Formulations for both large Commercial accounts as well as smaller entrepreneurs. We can provide Naturally compliant Formulations under the NSF, NPA, Whole Foods and USDA Organic Certifications. BS.Pharm Albany College of Pharmacy, Union University.
  • DavidDavid Member
    edited July 2015
    I use 50g "micro" batches sometimes in order to speed up some testing. However it is nothing for the beginner - you have to really know what you are doing. One remaining drop in the pipette can make the experiment worthless. Weighing in one beaker and transferring the material to another 
    beaker or 2 seconds without a cover means several kilos (%) are lost in "reality". Temperature gradients are steeper. As Bobzchemist nicely put it - it is like building a toy car with toothpicks. I would recommend 1 kg as well.
  • hello
     1/400 g   minimum batch
     2/let stand the final product a few days
    If the bubbles do not disappear, you have to play on the viscosity by decreasing the percentage of cocamide DEA or xanthan gum or surfactants.
  • BobzchemistBobzchemist Member, PCF student
    One of the nice things about making a 1 kilogram batch is that the math is so easy when your formulation is in % - just move the decimal point one place to the right, and you have the amount in grams that you need to add.

    I wonder if I'm dating myself with this approach to formulating? I'd be interested to know how many of you get why this used to be so much more important than it is now.
    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."
  • BarrowBarrow Member
    edited July 2015
    Thanks everyone for the comments and here I have some feedback. I made two 1 kg batches and the bubble problem is gone. This is how I did it:

    Batch 1
    • I dispersed xanthan into MPG (monopropylene glycol) in 1:3 ratio
    • I heated water to 95 degrees Celsius and transferred it into a variable speed blender.
    • While setting the blender to the highest speed I added xanthan into the blender in small amounts and blended it for 15 minutes continuously.
    • Then I added the rest of ingredients and heated to 75 degrees Celsius with gentle mixing after addition of each ingredient.
    • The final product did not have bubbles in it but there was a thin layer of xanthan paste on top of the mix and some clouds, which I thought to be some unhydrated xanthan, could be seen in the final product. However, these have gone after  1 1/2 to 2 days and  a nice thick and homogeneous product was produced.
    Batch 2:
    • I heated MPG to 50 Degrees Celsius and dispersed xanthan into it. Again the ratio of xanthan to MPG is 1:3.
    • I  heated water to 95 degrees Celsius and transferred it into a variable speed blender.
    • While setting the blender to the highest speed I added xanthan into the blender in small amounts and blended it for 30 minutes continuously.
    • Then I added the rest of ingredients and heated the mix to 75 degrees Celsius with gentle mixing after addition of each ingredient.
    • The final product was homogeneous and  no bubbles were present. No clouds could be seen either. It was success.     
    Thank you all for your comments.

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