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  • Emulsion Creaming

    Posted by ajw000 on August 20, 2021 at 12:06 am

    I am having difficulty with an emulsion creaming and weeping/sweating on top. 

    After emulsion a yellow substance (Likely lanolin) migrates to the top forming a thin yellow layer on the top of the product. The product will also sweat producing droplets on the surface. I’ve heard that increasing melt temperature and viscosity will help with this, but if I increase waxes too much more it makes the product more clumpy rather than creamy. I’ve tried adding more ceteareth-25 and it becomes more unstable. 

    Any suggestions for preventing creaming and sweating? 

    Please don’t pay attention to the odd order below, it pasted weird. Oil phase + water phase (180F) , fragrance + citric acid + phenoxy at cool down. I’m mixing with an immersion stick blender. 

    Water 50.49%
    propylene glycol 4.00%
    Potassium Sorbate 0.68%
    pvp 2.08%
    pvp/va copolymer 10.00%
    Petrolatum 12%
    Wax Lanolin 3%
    Cetyl Alcohol 2.50%
    Stearyl Alcohol 0.50%
    ozokerite 1.00%
    carnuba wax 7%
    Ceteareth 25 1%
    PEG-100 Glyceryl Stearate 2%
    Fragrance 2.50%
    Phenoxyethanol 1.00%
    Citric Acid 0.25%
    ajw000 replied 2 years, 1 month ago 7 Members · 39 Replies
  • 39 Replies
  • ketchito

    Member
    August 20, 2021 at 12:22 pm

    @ajw000 Petrolatum, lanolin, carnauba…they are heavy substances to be emulsfied. High viscosity of your emulsion might delay phase separation, but you’d still see things like creaming. I see you’re only using O/W emulsifiers, so I’d start by adding a W/O emulsifier as well, to make the emulsion more stable.

  • ajw000

    Member
    August 20, 2021 at 1:24 pm

    @ketchito

    I tried swapping out PEG-100 Glyceryl Stearate for straight Glyceryl Stearate, but that didn’t work either. Any suggestions on what type of w/o emulsifier to use? 

    Its not full creaming, its a yellow film that rises to the top, then it starts sweating on the top. 

  • ajw000

    Member
    August 20, 2021 at 1:28 pm

    The other strange thing is when I put it through stability testing: Heating and freezing cycles, it never separates, it stays strong. 

  • ajw000

    Member
    August 21, 2021 at 1:02 am

    @ketchito 

    I tried 2 different batches with water in oil emulsifiers

    1) adding 0.75% sorbitan stearate 
    2) adding 0.75% sorbitan oleate 

    Sorbitan stearate separated immediately 
    Sorbitan oleate didn’t stop sweating/weeping

  • ketchito

    Member
    August 23, 2021 at 3:37 pm

    @ajw000 I wouldn’t replace PEG-100 Glyceryl Stearate, but use both PEG-100 Glyceryl Stearate and Glyceryl Stearate. If needed, you could actually add another pair of W/O and O/W emulsifiers (like steareth-21 and steareth-2, like Unilever does in some formulas). Another approach would be to use both PEG-100 Glyceryl Stearate and Glyceryl Stearate, plus a polymeric emulsifier (like Sepigel 305).

  • bill_toge

    Member
    August 24, 2021 at 8:34 pm

    there’s an awful lot of potassium sorbate in there, that’ll not help with emulsion stability - plus, it’ll turn the product brown

  • ajw000

    Member
    August 25, 2021 at 3:33 pm

    @ketchito any suggestions on % to use for steareth-21 and steareth 2? I just tried steareth-21@1% and Steareth-2@0.5% and it had slight separation. 

    @Bill_Toge Thanks for the info. No issues with brown color, and I’ve tried test batches without Potassium Sorbate and had the same result. While Potassium sorbate may not be the culprit in this scenario, it’s good to know I can save some money on % amounts!

  • ajw000

    Member
    August 25, 2021 at 9:34 pm

    Correction, total separation after reheating and cooling. 

  • ajw000

    Member
    August 26, 2021 at 12:45 am

    +1% glyceryl stearate w/o steareth 21 or 2 and no results. 

  • ketchito

    Member
    August 26, 2021 at 2:34 pm

    @ajw000 I’d use something like that:

    PEG-100 Stearate     1.5-2.0
    Glyceryl stearate       1.5-2.0
    Steareth-2                  0.2-0.25
    Steareth-21                0.2-0.25

    I’d also cut Carnauba wax by half (or even better, replace it by a fatty alcohol, which give you consistency without impairing stability).

  • bill_toge

    Member
    August 27, 2021 at 8:56 pm
    speaking as an former employee of a subcontractor for Unilver/Alberto Culver, I can say that steareth-2 and steareth-21 were both included in their products at 2-5%, and we had no problems with emulsion stability
    (the granulation issues we had due to one of the resins precipitating above 35 °C in aqueous products, and the minimum filling temperature being 45 °C, were an entirely separate matter)
  • ajw000

    Member
    September 14, 2021 at 12:56 am

     I found a ratio that is more stable, however there is a bit of a problem. When I make a smaller batch without PVP/VA + PVP it is very stable. When I scale up to about 660 grams and add the PVP/VA the batch becomes unstable and separates. I’ve never experienced this before. 

    Has anyone ever seen this? I’m using those ingredients in the same manner (water phase) as I do with all my other products. 

  • ketchito

    Member
    September 14, 2021 at 12:05 pm

    @ajw000 Any reason why you have such level of PVP/VA and PVP? Hydrophilic polymers are not always welcomed in some emulsions.

  • ajw000

    Member
    September 29, 2021 at 11:35 pm

    @ketchito Hold for hair styling.

  • Joram

    Member
    September 30, 2021 at 11:49 am

    at what temperature are you adding the fragrance, plus it is also too much, sometimes if the fragrance does not blend in well it re-seperates

    does the product also apppear sliding in the container??

  • ajw000

    Member
    October 2, 2021 at 1:50 pm

    @Joram, I have tried batches substituting the fragrance for water, same effect occurs. No, it is a solid cream, no sliding in jar at room temperature. 

    The product does sweat after capping, water beads form on top of the product. I’m waiting plenty of time to make sure the external and internal temperature of the product reaches room temp. This, to me, points to the instability i’m experiencing, which makes me think its an oil/emulsifier issue. But I’m having difficulty locating it. 

  • ariepfadli

    Member
    October 3, 2021 at 7:30 pm

    Add more GMS or low HLB emulsifier

  • ajw000

    Member
    October 7, 2021 at 2:20 am

    @ariepfadli I did a trial with 

    1% Ceteareth-20
    1% PEG-100 Glyceryl Stearate 
    1% Glyceryl Stearate 
    Reduced Carnauba to 3%

    and made sure the HLB was balanced. 

    Still having separation on the bottom. 

  • abdullah

    Member
    October 7, 2021 at 3:35 am

    Can you send a picture of separation that how it looks. 

    For creaming xanthan gum helps

  • ajw000

    Member
    October 7, 2021 at 10:45 am

    @Abdullah See attached pictures. From the side it looks fine, but if you look underneath you see water pooling.

    As for viscosity and xanthan gum, I actually need to reduce thickness, it’s closer to a paste right now than a cream. There is a slight yellow film on the top of the product after it cools. Lanolin and Carnauba being the only yellow ingredients, this leads me to believe it is a stability issue, not a thickness issue. 

    I’m making sure the water and oil phase are mixed at at least 180f and mixed with an immersion blender until it reaches 145f to pour. 

  • ketchito

    Member
    October 7, 2021 at 11:41 am

    @ajw000 I usually heat to 75-80°C and keep the mixture at high shear for about 20-30 min (enough mechanical energy for difussion, colisions, etc.). Then I reduce mixing gradually while it cools (to let the emulsion system arranges), and finally remove mixing at around 45-40°C (from this, entrophy of the system will reach and equilibrium). Maybe you could try this to see if it improves.

  • abdullah

    Member
    October 7, 2021 at 3:04 pm

    @ketchito 30 minutes for what batch size? 

  • abdullah

    Member
    October 7, 2021 at 3:06 pm

    You need xanthan gum to prevent creaming. 
    If you have a film of oil on top increase your emulsifier. 
    If you want to reduce the viscosity reduce your oil phase or oil phase thickeners.

  • ketchito

    Member
    October 8, 2021 at 12:28 pm

    Abdullah said:

    @ketchito 30 minutes for what batch size? 

    Let’s say for a 100kg, but this also depends on your mixing speed and the ratio of your mixer diameter/container diameter, so the 20-30 min are referential (the main idea is to give the system enough energy to overcome crystalization while increasing interactions for later micellar arrangement).

  • ariepfadli

    Member
    October 8, 2021 at 3:09 pm

    ajw000 said:

    @ariepfadli I did a trial with 

    1% Ceteareth-20
    1% PEG-100 Glyceryl Stearate 
    1% Glyceryl Stearate 
    Reduced Carnauba to 3%

    and made sure the HLB was balanced. 

    Still having separation on the bottom. 

    Not enough, add span 80 or 60 2-3%
    GMS SE 1-2%
    And lower you petrolatum+vaselin and carnauba wax total

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