Something in the formula stops carbomer from forming a gel

Hello All,

There is something in my formula that stops sodium carbomer from forming a gel. I did a kick-out experiment and ended up with what I think shouldn't cause any issues, but I still can't make it thicken. Any advice is appreciated.
Formula:
A Aqua 74.55%
A Tetrasodium EDTA 0.20%
A Glycerine 2.00%
A Butylene Glycol 2.00%
A Propanediol 1.00%
B Jojoba oil 6.00%
B Shea butter 3.00%
B Petrolatum 3.00%
B Tocopheryl Acetate 0.20%
B Tocopherol 0.50%
B Sorbitan Oleate 1.00%
B Glyceryl Oleate 4.00%
B Polysorbate 20 1.50%
C Sodium Carbomer 0.30%
C Paraben DU/phenoxyethanol 0.75%

I tried sodium carbomer, ultrez 20 and ultrez 30 (when last two were used I neutralised it with TEA). Nothing works. 

Comments

  • Stupid question, but did you check pH before neutralizing? And during? If you add too much TEA you will break the gelling if pH is too high. If pH is too low again will not gel.
  • @Dirtnap1please let's respect each other @ngarayeva001 actually if can not fînd any ingredient wich cause the problem really difficult your problem.
  • Hello All,

    There is something in my formula that stops sodium carbomer from forming a gel. I did a kick-out experiment and ended up with what I think shouldn't cause any issues, but I still can't make it thicken. Any advice is appreciated.
    Formula:
    A Aqua 74.55%
    A Tetrasodium EDTA 0.20%
    A Glycerine 2.00%
    A Butylene Glycol 2.00%
    A Propanediol 1.00%
    B Jojoba oil 6.00%
    B Shea butter 3.00%
    B Petrolatum 3.00%
    B Tocopheryl Acetate 0.20%
    B Tocopherol 0.50%
    B Sorbitan Oleate 1.00%
    B Glyceryl Oleate 4.00%
    B Polysorbate 20 1.50%
    C Sodium Carbomer 0.30%
    C Paraben DU/phenoxyethanol 0.75%

    I tried sodium carbomer, ultrez 20 and ultrez 30 (when last two were used I neutralised it with TEA). Nothing works. 
    Was the formula well emulsified, and not separating before adding carbomer?
    I believe it has too many oils and little sorbitan oleate and Tween 20.

    Try with a ready made, commerical emulsifier.

    Also, try without EDTA
  • edited November 27
    @Dirtnap1, It’s SODIUM carbomer. It’s a preneutralised form, so no neutralization is required. And I specified that I used TEA to neutralize versions with ultrez 20 and 30. Neutralise means bring pH to 7.
  • @Gunther, the point is actually to figure out this combination.  HLB is balanced, product emulsified well. There are sorbitan oleate, 4% of glyceryl oleate and polysorbate 20 (to balance HLB). The reason for such a combination is that I don’t need fatty alcohols and silicones for it, and (if exclude butters and petrolatum) it can be made using cold process.
  • @Fekher - I think you are misreading the tone of @Dirtnap1 response. I don't think they were saying the question was stupid. The phrase "stupid question" is an idiom in English which is meant to be self-deprecating. It's not used as an insult.


  • That's usually an electrolyte problem so leaving out the EDTA would be a first good experiment
  • Thank you @Perry. This formula is what is left from the initial one. I thought I excluded everything suspicious. You are right, I will try knockout experiment. This must be something in the waterphase.
  • An update. I did a knockout experiment. It's not the waterphase. I excluded heavy butters (petrolatum and shea butter) and it gelled. I don't know what to think. I didn't know that butters can impact rheology.
  • How about changing the order of addition, Sodium Carbomer before oil phase.  And then the rest of the things. 
  • I just thought that mixing oil phase with gelled waterhpase might have an adverse effect on emulsification... Am I wrong?
  • You may neutralize the carbomer after emulsification... if you neutralize it before, you may have air bubble entrapment due to high viscosity

  • edited November 28
    How about adding the carbomer to the heated oil phase?
    If I don't make a Geltrap or HIP W/O emulsion, I practically always put polymers in the oil phase and never had this problem.
    I don't know if it helps, but maybe it's worth a try?
    Good luck!

    Edit: in a Geltrap or HIPe the gel has to be formed before emulsification and has no adverse effect on the emulsion. I prefer adding polymer to oil phase in other formulations because it's quicker.
  • @jeremien
    Where do you read that ngarayeva001 puts the TEA before emulsification?
  • @Doreen can carbomer gel the oil ??? and do you neutralize it ? wha process do use for that?
  • Doreen ... as i read "gelled waterhpase", i thought that he have already neutralized it before emulsification... it may be a wrong interpretation
  • Guys, I am using Sodium carbomer. It is a preneutralised form of carbomer that doesn't require any TEA. You simply put it in your water leave it for 10 minutes to hydrate and it turns into a gel. I saw it in many Chanel products and found it on lotioncrafter. It's a great thing to use in the cool-down phase, because when you add it to the vortex you see the result momentarily, which allows controlling the thickness of the product, so I really recommend to order a small pack if you never used it.

    Carbomer aside, I managed to make it work when I knocked out shea butter and petrolatum, which left me very confused. I didn't know that oil can affect rheology.
  • edited November 28
    @ngarayeva001 yes sodium carbomer is a product of hydroxide sodium and carbomer so it is neutralized and did not need a neutralizer.
    About Shea butter i'am sure that it dosen't break gel cause i had some experiences about that.
  • edited November 28
    @ngarayeva001
    Not the sodium carbomer, but the Ultrez 20 and 30 where you used TEA to neutralize, I think some people here write about those.

    @Fekher
    No carbomer doesn't gel the oil phase. I put polymers in the oil phase (when the formula allows it) because this way they don't hydrate right away and dispersion can be better and quicker.

    @jeremien
    When ngarayeva001 writes about a 'gelled waterphase', she is answering Chemist77. She asks that IF you would put it in the water phase wouldn't that have an adverse effect on emulsification.
  • @ngarayeva001 I would be very interested to know the results in case you change the order of addition. 
  • @Chemist77 I will write an update once I try it.
  • I would try adding the sodium carbomer to the oil phase.
  • Fekher said:
    @Dirtnap1please let's respect each other @ngarayeva001 actually if can not fînd any ingredient wich cause the problem really difficult your problem.
    I meant stupid question on my part. No disrespect at all on my part. 
  • Have you tried using something along the lines of Pemulan TR-1 (2) in place of the sodium carbomer? You mentioned butters, so may be worth a shot.
  • @Dirtnap1, I don’t have it unfortunately. Both sodium carbomer and ultrez 20 worked when I excluded butters and left only jojoba oil. But surprisingly enough a moisturizer with 10% of jojoba oil only feels greasier than a mixture with shea butter and even petrolatum totalling 12%. I will try to add carbomer/ultrez20 to the waterphase to see if there’s any difference.
  • @Gunther, the point is actually to figure out this combination.  HLB is balanced, product emulsified well. There are sorbitan oleate, 4% of glyceryl oleate and polysorbate 20 (to balance HLB). The reason for such a combination is that I don’t need fatty alcohols and silicones for it, and (if exclude butters and petrolatum) it can be made using cold process.
    You can use PEG-50 shea butter instead of shea butter, which is water soluble and mineral oil instead of petrolatum. This way you can turn your formulation process to cold process. 
    Regarding your issue with gelling, have you tried to increase the sodoim carbomer percentage? I'd suggest to try 0.5%, 0.7% and 1% and see if the problem persists. 
  • Thank you @em88. I will try PEG-50 shea butter. It actually tends to "soap" in serums but let's see how it's going to work in this system. 
  • edited November 29
    @ngarayeva001 I hope you get it to stabilize.

    If it works but soaps a bit, you could add a dash of dimethicone to reduce the soaping effect.

    If you're going for a silicone-free version you could add Plantasens® Olive LD / Softolive / Fision® EcoSil

    For a hobby-crafter, I only know of one retail-supplier of this; http://www.farmaciavernile.it/index.php?page=shop.product_details&category_id=9&flypage=flypage.tpl&product_id=3291&option=com_virtuemart&Itemid=65&vmcchk=1&Itemid=65

    Edit: (I don't know which of them it actually is... My guess is Plantasens, but I am not certain).
    Dabbling Formulator — Qualified Cosmetic Safety Assessor — experienced in claim substantiation & EU regulatory affairs.
  • @ngarayeva001
    I don't think 1.5% Polysorbate 20 will be enough to emulsify 12% oils, 4% glyceryl oleate and 1% sorbitan oleate.

    BTW is that sorbitan oleate actually Polysorbate 80?

    IMO you'd be better off with a ready-made, commercial emulsifier that both emulsifies and thickens.
  • @Gunther, maybe I am missing something, but I have 3 emulsifiers (6.5%) in this formula. The only purpose of polysorbate 20 is to bring down HLB of the emulsification system (to make it the same as the total hlb of the oil phase). Sobritan oleate is a liquid low hlb emulsifier. Same as glyceryl oleate. There’s no polysorbate 80 at all. I have commercial emulsifiers, both conventional and polymeric but I am trying to get a particular sensorial that I will not get with waxy commercial blends. The reason why I am avoiding polymers is that I am going to use this formula as a base to add tetrahexyldecyl ascorbate. Sodium carbomer tolerates it, but Sepinov, Aristoflex, Sepiplus 400, Emulthix and couple others stubbornly lose viscosity. And I am trying to avoid using fatty acids in this formula.
  • Hello All! An update:

    I changed shea butter to PEG-50 Shea butter and Squalane (6% of shea butter replaced by 4% of squalane and 2% of PEG-50 Shea butter). I also used a mixture of Ultrez 20 and Sodium Carbomer (0.3%+0.2%). Ultrez was added to the water phase and Sodium Carbomer after emulsification and neutralization of Ultrez. I suspect I can just up Ultrez to 0.5-0.6% and will get the same result. The great thing about sodium carbomer is that it can be used to "fix mistakes".

    So, I got a base with a very nice light texture (cold process and no tackiness that is so typical for polymers) and no silicones. I added retinol liposomes and tetrahexyldecyl ascorbate in it (no loss of viscosity). I usually use silicones, but I didn't want anything in the formula that can potentially interact with the actives (liposomes are slow release already, so I didn't want to add silicones that in theory might slow down the absorption of retinol).

    Thank you all very much for your help. The formula if you want to use it:

    8.61
    Phase INCI %
    A Aqua 70.75%
    A Tetrasodium EDTA 0.20%
    A Glycerine 1.00%
    A PEG-50 Shea butter 2.00%
    A Butylene Glycol 2.00%
    A Ultrez 20 0.30%
    A Propanediol 1.00% HLB Weighted av HLB calc
    B Jojoba oil 4.00% 6 45% 2.68
    B Squalane 4.00% 12 45% 5.36
    B Tocopherol 0.10% 6 1% 0.07 Oil phase HLB
    B Tocopheryl Acetate 0.75% 6 8% 0.50
    B Sorbitan Oleate 1.00% 4.3 14.3% 0.61
    B Glyceryl Oleate 4.00% 3.5 57.1% 2.00
    B Polysorbate 20 2.50% 16.7 35.7% 5.96
    C Sodium carbomer 0.20% 8.58 Emulsifier HLB
    C Retinol liposomes 2.00%
    C Tetrahexyldecyl ascorbate 3.00%
    C Bisabolol 0.20%
    C Paraben DU 1.00%
    C TEA  
  • Congratulations! :smile:

  • edited December 3
    @ngarayeva001
    So you left out the petrolatum, I see. Did it still give problems?
    Congratulations by finding a way around it! :+1: 
  • @Doreen, petrolatum did give problems. I could overcome it by increasing level of rheology modifiers, but it lead to the peeling of the ready product. So I decided to skip it. It actually makes sense as it's a very lightweight base. Great news is that rheology modifiers I used abobe can tolerate tetrahexyldecyl ascorbate, which broke viscosity of both Sepinov EMT10 and Aristoflex AVC.
  • @em88, thank you for the idea with PEG-50 Shea butter. Btw is doesn't cause soaping.
  • edited December 4
    @ngarayeva001, glad it helped. 
    I was wondering why did you chose squalene. Why not mineral oil?
    Have you tried using only sodium carbomer at 0.5%?  I'm asking because you have 20 ingredients in you formulation which will slow down the production of this product. 

  • @em88 I am a hobbyist, and I learn by analyzing benchmark products and experimenting. The reason why I used squalane is pretty much because Chanel uses is in two moisturizers that I like. I did my research about it and it sounds like a good emollient. Please let me know if you think it doesn’t add anything because I am running out and it’s expensive in the UK where I live. 0.5% of sodium carboner in this particular formula causes peeling of the final product. I might try .5-.6% of ultrez when experiment next time. As I said sodium carbomer is great to fix mistakes. Ultrez 20 is better on its own (silkier feel). Btw sodium carbomer is very often used with aristoflex AVC but I have never seen it as the only rheology modifier.
  • edited December 4
    @ngarayeva001
    I can tell you right away that squalane doesn't add anything. It's a claims ingredient mostly.
    Carbomers (pre-neutralized or not) can be used as only gelforming polymer, I've seen it before. It depends on other excipients and what you want qua sensorials.
  • Thank you @Doreen. Crossing it out of my "to buy" list. It is outrageously expensive, and substance over form, it's just an emollient. I liked it, because it's rather light, but there are light oils at a greater availability.
  • @ngarayeva001, I don't know why when I was reading sodium carbomer, I was always thinking that you were using sodium polyacrylate. My bad. You should try sodium polyacrylate as well. 
    I'd still go for mineral oil, it is cheaper, it has a nice skin feel and it is as well an emollient.  https://www.ncbi.nlm.nih.gov/pubmed/22994201

  • @em88 I have an emulsifier based on sodium polyacrylate (ViscOptima). I absolutely like it, and it can thicken pretty much anything (except for Sodium PCA). However, I prefer carbomers for this product because it provides much lighter feel. Thank you for the info about squalane. I bought it long ago, and that was not something I was questioning. I will just replace it to mineral oil.
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