Help! Problem with Ceteareth 25 - Cosmetic Science Talk

Help! Problem with Ceteareth 25

edited July 13 in Formulating
Hi Everyone 

I have a problem with a formulation about Hair water based pomade and I would like you to help me solve it 

The problem is that when i heat the mixture in water with the ceteareth 25, the Ceteareth 25 isn't dissolved completally but instead becomes a translucent mass floating on water

The presentation of the ceteareth is in pellets like NaOH, not powder and the msds says that the ceteareth is completely soluble in water 

Maybe if i pulverize the ceteareth in a mortar and I add it to the hot mix, Would completely solubilize? or if i increased the amountthe water amount the ceteareth works better ? (water 60% aprox, C-25 21% aprox in formulation) 

heating temperature = 60°C

Thanks

Comments

  • Couple of issues:

    (1)  C-25 ... 21% ... is that correct or did you mean 2.1%?  If 21% is correct, then that's the major part of your problem ... you only need about 2% C-25

    (2)  Temp = 60C ... trying upping your temperature to 70C to 75C.

    But, if you are using 21% C-25, that's your problem.
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • Yes, the c-25 is 21% in the mix 
    Thanks @MarkBroussard , I will try it 

    The goal is producing something like this:
    https://www.maggardrazors.com/wp-content/uploads/2017/01/Hey-Joe-Strong-genuine-hair-pomade-100ml-2.jpg

  • edited July 13
    Search this forum with Ceteareth-25 and you will get all the information. I remember a long discussion on this and few including me have posted almost complete formulation. The product you posted the picture of is what I developed too. And it has indeed more than 25% Ceteareth-25.
  • It would help if you posted the full LOI of the benchmark formula.
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • @MarkBroussard  @Chemist77  Here is the formulation

    Ingredient                         %

    Water                                59,1
    Propylene Glycol                2,7
    Benzil Alcohol                    0,5
    Polysorbate 20                   2,0
    PEG 7 Glyceryl Cocoate      1,7
    Vegetable Glycerin             1,4
    PEG 40 castor oil                0,8
    Polysorbate 80                   1,3
    Fragance                            1
    Pvp k30                              3,5
    Ceteareth 25                      25,0
    Silicone oil                         1,0

    Today i increased the heating temperature to 75°C in a Home water bath ( I don't have a lab water bath) and the ceteareth remains undissolved completely

    I tried mix  with a mechanical mixer, the ceteareth dissolves completely but too much foam is formed, and the silicone oil does not function as an antifoam agent

    The ceteareth stayed like:

  • I have not ever worked on a formula like this, so I can't offer any more advice.  Is this a formula you developed on your own, or are you trying to replicate a formula you found fully-developed from a formulary?
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • edited July 14
    @MarkBroussard @Chemist77
     i trying to replicate a formula i have fully developed from a formulary. The goal is producing something like this:
    https://www.maggardrazors.com/wp-content/uploads/2017/01/Hey-Joe-Strong-genuine-hair-pomade-100ml-2.jpg

    But the problem is that the ceteareth isn't dissolved completely in water and if i mix with a mechanical mixer, a lot of foam is formed but the ceteareth is totally dissolved 

    So i think that maybe if i use an anti-foam agent could work but I don't know what agent could use in this case so that it does not involve any risk in its application
  • edited July 14
    Add upto 10-15% glycerine and propylene glycol combined to the batch and then process everything at not less than 85C.
  • Hey @Chemist77 @MarkBroussard Thanks for the advice, these were very useful.

    I have achieved the desired consistency in the final product. Apparently, the problem was the heating temperature, raise the temperature to about 85 ° C, and I have separated the mixture into two phases, which after being brought to that temperature I mixed them and worked well

    But, I have one last question:

    In my formulation, I have reduced the water level slightly, increased the C-25 and maintained the percentage of benzyl alcohol in the mixture (2%). Understanding that benzyl alcohol works as an antimicrobial agent and can also cause skin irritation, Don't you think the percentage is high? Could it involve any risk to the skin?

    I thought of reducing this percentage to 1% (0.5% of Benzyl Alcohol and 0.5% of another preservative, Maybe, Phenoxyethanol) But I don't know and I would like to know your opinions about it

    Thanks so much!
  • The concentration for benzyl alcohol used for topical formulation is up to 2%, but benzyl alcohol is active in pH below 8, if I'm not mistaken, and the optimum pH should be up to 5
  • You might want to try Benzyl Alcohol + Dehydroacetic Acid ... it's a well-established, commercially available blend ... use at 1% and you should be fine.
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • edited July 19
    I don't recommend dehydroacetic acid because it is chemically quite active and is able to decompose salts (double replacement reaction). For example potassium glycrrhizate + dehydroacetic acid -> some kind of precipitate and unknown byproducts. Just 0.5% of dha ruined a 40% solution.

    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • And what salts do you see in this formula?
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • Just for information: we have used  0.75 and 1%  benzyl alcohol (passed USP 51) at Ph up to 10 in the presence of high levels of Ca CO3.
  • I wasn't talking about this formula specifically.
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • I see ... a general comment.  So, Benzyl Alcohol + Dehydroacetic Acid would work just fine in this formula.
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • edited July 19
    @MarkBroussard i will try that combination , Thanks 
    But is the percentage of benzyl alcohol in the formulation okay? There is no risk?
    And talking about the preservation and stability of the product, this was what was obtained:



    I take a sample of the container, exposed it to the air, to the interperie and now it looks like this:



    Is this normal? Or is there any stability problem?
  • Seems to have gone from translucent to opaque, so yes, there appears to be a stability issue. Opaque usually means formation of crystals.
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • Agree if you look closely you can see crystals formed.Put it under the scope to be sure.
  • edited July 19
    @Belassi @DRBOB@VERDIENT.BIZ
    Here is the new formulation

    Ingredient                         %

    Water                                47,1
    Propylene Glycol                2,0
    Benzil Alcohol                    2,0
    Polysorbate 20                   1,9
    PEG 7 Glyceryl Cocoate      6,0
    Vegetable Glycerin             4,0
    PEG 40 castor oil                0,7
    Polysorbate 80                   1,0
    Fragance                            0,5
    Pvp k30                              3,0
    Ceteareth 25                      30,0
    Silicone oil                         1,0

    Any suggestions to avoid crystallization?
    I clarify that if the product remains in the open container does not happen, only happened when you take a sample there and leave it outdoors
  • I would do a knockout based on the indoor/outdoor reaction.I don't see anything obvious!
    • Forgot to mention BA is too high as all you need is 1percent.
  • edited July 19
    DRBOB@VERDIENT.BIZ 
     Knockout experiment? sure!

    If anyone knows that could be causing the crystallization in the formulation, I would be very grateful if I discussed it and help me to get a solution

    I clarify again, this only happens if I leave something of the sample to the interperie for approximately 24 hours



  • I was thinking, and maybe what happened was a phenomenon of oxidation in the product and this is why its coloration became opaque?

  • edited July 20
    The silicone oil and PVP in there are going to cause turbidity, read my previous comment. The glycerin and PG content has to be between 10-15% minimum. Chuck out the cocoate also along with the silicone oil. Optmize PVP.
  • @Chemist77
    The turbidity or the product becomes opaque when I withdraw it from the plastic container in which it deposits and expose it to the open air for a long time (24 hours), the product is still translucent in the plastic container

    Is it because of silicon oil and pvp this phenomenon?
  • Oh, I see. Well, why are you doing that? I don't see that there's anything to oxidise. The fragrance will evaporate and maybe the benzyl alcohol too and it will lose water ... it would be surprising if nothing happened wouldn't it? That class of inertness is reserved for McDonald's hamburgers.
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • Your formula includes Polysorbate 20, Polysorbate 80 and PEG40 Castor Oil ... why all 3 to solubilize 0.5% fragrance.  You might try cutting out a couple of these.

    I would leave the Cocoate in as it can aid in wash-out, but you could probably cut that down to 2%.
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • Thank you so much for your advice, I will try all that and tell you what happened.
    See you later
  • edited July 20
    @Belassi ;Do you consider that the color change (translucent to opaque) is something "normal" in this formulation?
  • I'm sorry I can't comment further, this is a product type I don't have any experience with.
    Design of anti-aging creams, gels, and serums; shampoos; and therapeutic cosmetics. In-house label and box design capability.
  • if it doesn't happen in a closed container, the product is most likely losing water and drying out in the air

    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
  • edited July 21
    Exactly @Bill_Toge , it only happens when I leave some of the sample outdoors

    But, is there any way to reduce this?
  • Start your formula with C-25 @25%, glycerin/pg combined at 15%, preservative, fragrance. You will get a clear and stable product, now you can do the reverse of knock out trials. Add one ingredient at a time and see how it behaves in the formula, mind that silicone or any other polymer like PVP is definitely going to affect the clarity of the solution.
    Good luck.
  • The most simple solution to the product turning opaque when left uncovered is to put the cap back on the jar right after you have used the product.  

    No offense, but leaving the cap off is kind of like peeling bananas and leaving them on the counter and wondering why they keep turning brown.
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • jaja No problem @MarkBroussard ;But if I wanted to know that in case it is lost from moisture, how could I avoid it?

    well, apart from having the container closed
  • I don't know that this can be avoided per se ... to reduce it, you would have to include an ingredient that would bind the water to slow the evaporation.  

    You would have to evaluate the value to you of doing that.  

    Plus, you do want the water to evaporate when the product is placed in hair for the hold to develop.
    Chemist/Microbiologist formulating in the Organic & Naturals arena under ECOCert/Natural Products Assn/Whole Foods/National Organic Program guidelines focused skincare & haircare products. 

    Provides Formulation Development and Lab-Scale Contract Manufacturing Services.  See website for details www.desertinbloomcosmeticslab.com

  • edited July 23
    Thank you all for your advice

    I did what he recommended and the appearance has improved a lot, apparently it is also normal to dry the surface of the product outside the container for a long time, but it isn't a stability problem
  • @Chemist77 @DRBOB@VERDIENT.BIZ  @Bill_Toge  @MarkBroussard  @belassi @em88

    Hi everyone, it's me again
    I have been testing my product with myself and some of my friends
    They tell me that apparently the fixation of the pomade is a little bad and that after washing still leaves the feeling that it is in the hair. With the above I have some questions

    Is it better to use pvp k 30 or k 90? What is the maximum allowed level of pvp in a formulation like this? What could change in the formulation to make the washing a little easier?

    Thanks so much
  • edited August 10
    :smiley:
  • Aloha) silicone which you use in the product is not easily washed off) 
  • hello every one
    i recommend new hair pomade/ wax formula 
    Ceteareth 25        25%
    Propyline glycol    5%
    PEG-400               2%
    Kathon-CG           0.1%
    Tween-20             1%
    Perfume                 0.3-0.4%
    DM Water              Qs to 100 %

    Process - 1. Ceteareth-25+PG+PEG-400 Heat- 65-70@C
     2. DM Water Heat 85-95@C 
    3. Mix both Phase or Continuous heating or mixing 90-95@C Ceteareth-25 completely disolve. its very stable formula 
    4. perfume+ tween-20 mix properly
    5. than add main mixer perfume blend or kathon-CG or filling to heat material in jar. 
    very stable formula.

    any outher help related in cosmetics formulation, please feel free contact.

    thanks & Regards,
    Somdatt Tyagi
    R&D Scientist 
    Nature Essence P Ltd.


  • hey @somdatt
    What ingredient in your formulation is responsible for fixing to the hair?

    Could you help me with the questions I ask? Thanks so much
  • Hello everyone
    I wanna commented that I have been able to improve  the "wash" in the fomulation and that apparently doesn't matter that amount pvp wich that attempt to add, the fixation is maintained medium to soft, therefore a combination with other fixing polymers must be able to increase the Fixing of the Product, now a new trouble has appeared to me.

    The fragrance next to the preservative should be added at a temperature of approximately 50 ° C but at that temperature and the sample is too gelled so it is very difficult to pack and much of it is lost (it remains stuck in the beaker)

    I think the solution could be to cut ceteareth -25 down to 5-10%

    I would like to know your opinion about this "possible" solution

    Have a nice day
  • If you add the fragrance at a temperature over 50C, you won't completely destroy it, you'll just evaporate more of it than you would if you added it at a lower temperature. This will raise the cost a bit, which is something that most of us try hard to avoid.

    But...if you have a formula that is working in all other aspects, it might make sense to add some additional fragrance at a higher temperature (to compensate for the increased evaporation) rather than start changing the functional ingredients.
    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."
  • edited August 21
    @bobzchemist Thanks so much
    About the preservative, I am using benzyl alcohol (0.5%) and would like to know if at a temperature of 70 ° C this would lose antimicrobial activity.
    According to the handbook of pharmaceutical excipients, the boiling point of this is 204 ° C and its flash point is above 100 ° C so I think this should not lose any of this in the product

    If it is correct what I think, then there would be no problem in adding everything to 70 ° C (Temperature in which packaging is easy) taking into account your advice on an extra fragrance, Right?
  • the flash point is the temperature above which a substance can spontaneously ignite: the vapour pressure is a measure of how readily it will evaporate

    having said that, from personal experience, I've never had an issue with benzyl alcohol at that kind of temperature
    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
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