Cloudiness in liquid soap...

I have some liquid soap that I have made that has some cloudiness in the top 1/2 inch or so of the containers.  I have researched the issue and found two possibilities.  One might be that even a slight amount of "superfatting" the oil phase may cause this and that "superfatting" is not recommended in this type of formulation.  The other option might be that the cloudiness is coming from the fragrance not totally being emulsified into the liquid soap.   My formula is not "superfatted" and takes into consideration the 90% of the Potassium Hydroxide.  Now, another factor is pointing toward the fragrance issue and that is that a couple of the scents (fragrance oil) have no cloudiness in them!  Here is the typical ingredient list so that I make sure there aren't any other possible issues!

Ingredients: Water, Cocos Nucifera (Coconut) Oil, Oleic Acid, Ricinus Communis (Castor) Seed Oil, Potassium Hydroxide, PEG-150 Pentaerythrityl Tetrastearate, Glycerin, fragrance, Caprylyl Glycol, Phenoxyethanol, Hexylene Glycol

It was suggested using polysorbate 20 for the fragrance issue.  Do you have any other options or suggestions?

Amount listed were 1-20% from the MSDS sheet.  Do you have Any suggested amounts or ranges?

Is it better to do this when product is still warm from production or can this be used at room temperature?

Should the fragrance and Polysorbate 20 be mixed together before being "homogenized" into the mixture?

Thank you in advance for any suggestions or information you can provide!  :)

Regards, David
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  • I have been working with a bottle of liquid soap and adding small amounts of Polysorbate 20 to the batch and stirring it then letting it settle.  The first time I used a small amount, the second a bit larger and more today.  The cloudiness seems to be all over now but much finer than before and the top half inch of cloudiness is there but less obvious.  After today's addition, I hope I get better results but I won't know until tomorrow.  I've been searching for more info on the use of Polysorbate 20 (and 80) and have found a few things but most are from soapmaking boards or blogs.  I would prefer to get my info from a cosmetic chemist who works with formulas and has the background and knowledge needed to use the best approach in making any of my products.  The late Maurice Hevey was the first chemist I encountered on a message board and I quickly saw the benefits then Perry came along and I eagerly jumped aboard the ship!  If any of you have any input that are willing to share I would greatly appreciate it.  I want to make the best product I can! 
  • letsalcidoletsalcido Member
    edited March 20
    I’m developing a “natural” body wash with a castile soap base like yours, and having similar issues.

    My take on this is that you’re on the right track. But there doesn’t seem to be a straight answer to fix your formula. You’ll have to experiment, as all ingredients will have a different effect on micelle stability.



    These two bottles are from a “failed” experiment of a peppermint and menthol body wash.

    Here’s what I did: I tested 1:5 oil to PS20, at 1% essential oil in pure castile soap. This created a perfectly clear mixture. I tried a 1:2, also clear but it took longer to clarify. I decided on 1:2 since eventually I would achieve enough clarity and I only had a small sample of PS20.

    I did a 500g batch (300g is castile soap) and added my fragrance and PS20. All good till then, fairly clear after mixing. I could tell when left at rest it would completely clarify. I added 100ml of 5% salt solution. It broke and turned creamy/white. I continued with my recipe and tried to thicken it more with  Cocamidopropyl Betain. Still white.

    I did another 500g batch, but instead of adding the sodium first I added the coco(...) betain. Broke before I added the sodium.

    So I tried to fix it. I figured that the electrolytes and anything that may alter the viscocity of the soap (preservative, type of essential oils, menthol) is actually putting ionic stress on the micelles and eventually causes it to break. But this is not irreparable, I tried to fix one of the 500g batches and basically halved the concentrations of essential oil and polysorbate by doing 250g of my broken batch and 200g of fresh castile soap + 50g of other stuff. That immediately turned clear again, and It became thicker too (hello micelles!). I added glycerin (10g) and made it even clearer, but more watery. Added the required Phenoxyethanol amount to get it to 1% and i turned a bit thicker but not quite there. So I adjusted it further with Coco(...) Betaine (5g?) and 1g of salt in Q.S. water. Left bottle in the pic was the first fixed batch. The one on the right, I did basically the same procedure but I tried adding a tad bit more salt (bad idea) and it turned a bit more opaque but still seems to be that it will be stable and won’t separate, it’s just not emulsified fully like the clear one.

    Another pic of another creamy looking batch I fixed this morning which has orange essential oil (citrus oils are hard to get clear apparently):



    What I learned from this:
    * Anything that alters the viscocity of your soap (interacts with micelles) can break the emulsification of your essential oils and make it look creamy.
    * even without essential oils, your soap will turn creamy and slimy if too much sodium is added. 
    * if it looks creamy and has oils in it, it will separate eventually
    * Each essential oil is different and will behave differently.
    * Any other actives in your formula can destabilize it.

    If you are set on the preservatives and fragrance you want to use, I recommend doing a “titration” to find the balance. You’ll notice that you may achieve a peak thickness before adding a single drop of anything and it breaking. 


    If you’re curious, my base castile is 60% Olive, 40% Coconut, approximately 1:4 oil to water ratio.

  • WOW!  Thanks for all of this "info" and observations and pictures!  It is becoming a bit more "clear" (pun intended) as to what all of the aspects are to take into consideration!   I am using essentials oils and also using fragrance oils and sometimes a combination of both so that should play a role in all of this as well!  I'm going to go over what you posted and reply when I have time to "absorb" (pun intended) all of this!  Seriously, I really appreciate your input and I am grateful for your help!   David

  • We successfully do a lot of liquid soap in large vats. A few points based on the comments above:
    1. Why would you add a preservative? Liquid soaps are self-preserving and are included in the ISO 29621 Cosmetics — Microbiology — Guidelines for the risk assessment and identification of microbiologically low-risk products. Under our local GMP regulations, we have Challenge Tested all new formulations and the results are excellent.
    2. During the in-process QC, our QC Manager does a  simple "saponification test" to ensure that the saponification is complete. This is recorded on the BMR.
    3. Our philosophy is "keep it simple." We make large batches of liquid soap bases using various combinations of oils, or just simply a coconut oil base, and an extra-virgin olive oil base. Once a batch is completed, we store for two weeks in jerrycans, then our QC Manager does a range of QC tests, and if OK, release the batch to our production crew.
    4. I can't comment on fragrance oils because we never use them.
    5. Yes, certain essential oils can cause cloudiness and increase viscosity. My advice, learn to identify these and avoid them. Also, in some cases, cloudiness may appear initially, then after a few days, clear.
    6. In the production phase where EO's are added, we leave the mixed batches sitting for 1-2 hours, and our QC Manager will evaluate before allowing the production crew to proceed with bottling.
    Hope the above is helpful. And my main advice is to keep it simple, the more gunk added is likely to increase clarity problems.

    Below is a pic of a nice clear liquid soap in our vat, ready to go into jerrycans.





    Dr. Mike Thair
    Cofounder & Chief Formulator
    Indochine Natural
  • letsalcidoletsalcido Member
    edited March 20
    Thanks for your input @mikethair!

    To address some of your comments:

    - I understand that soaps are “self preserving”, but it will depend on concentration. In the bodywash I’m formulating I must have < 12% soap (1kg of oil in a 5kg batch, not counting the glycerin that’s the byproduct and it’s only 60% of the final product). If you take a look at most shampoos and body washes they do use preservatives given the extremely high water content. I in fact I had a batch with only 0.2% citric acid and 0.1% EDTA (bad idea, it gelled like crazy) that had bacterial colonies growing on it after 2-3 weeks (easily distinguishable because it had gelled and it looked like a petri dish). Also, the pH of my liquid soap routinely tests ~5.5 (perhaps I’m using the wrong kind of strips, and haven’t invested in a pH meter).

    - Castile soap is easy to make, but in its pure form is very strong. It also lacks the cosmetic luxury that some people are looking for (thickness, natural fragrance, humectants). So I’m not trying to sell plain castile soap, but rather a more natural body wash. 

    Here’s my finished liquid castile soap. Pretty good clarity, but it’s hard to enhance it for that “luxury” feel.

  • letsalcido,  Your first two pics show one on the left side which looks quite nice to me even though you list them as "failed batches"!  The second pic shows two batches that are very similar to mine in color and they are fairly clear but not 100%.  The third attempt of mine yesterday on that one batch (that was made by adding fragrance oil to a "cold" batch that was 100% clear before adding the fragrance) had "cloudiness" at the top but now has it throughout the bottle but less dense and does look a little better today but I only put in the Polysorbate 20 in multiple drops each time just to see what would happen! 
    Mike, I think we are going for different markets so my customers are more concerned about consistency and skin feel which is why I chose the PEG-150 Pentaerythrityl Tetrastearate which has worked quite well and so far hasn't been affected by the addition of Polysorbate 20.  As letsalcido said, it is going to be something I will have to make work in whatever way I can find from batch to batch and fragrance to fragrance.  Letsalcido also mentioned using sodium (I am assuming as a thickener) but is one option that didn't appeal to me. 
    I would like to keep my products "all natural"  but that option isn't always the best option for the customers desire for just the right consistency and skin feel!  Interesting hearing about both of your production techniques.  I make mine early in the day, giving it some chance to sit in it's gel state which occurs fairly quickly with a fatty acid in the formula then it left to sit for a bit then water is added, left overnight then homogenized the next day with the addition of fragrance or essential oils.  Hopefully I can work this out and get that one "esthetic" part of the formulation correctly for a product that already does quite well as it is!  Thanks again, guys for your assistance! Letsalcido, nice earrings!  ;)
  • @David08848 thanks for the compliment and sorry if my redaction was confusing! The two green washes are made from a failed batch that looked extremely creamy. I split that batch in half and fixed them separately with slightly different amounts of sodium. Those two bottles are the result. 

    Same thing with the orange ones. Except I followed the same process for each so they look the same.

    I would say that sodium is “natural”. I actually am using sea salt. I’m sure there may be some other minerals in there, but overall it should give consistent results. I would think that marketing your body wash as containing “sea salt” or “pink himalayan salt” could be attractive to the consumer. You’d just need to adjust it to each type of salt and make sure it doesn’t react in an unexpected way. of course, you can thicken with something else. Just my 5 cents.

    In terms of process, I have been very impatient and mix all my additives to the castile soap within 5-15minutes from each other. I’m hoping to find a “fool proof” recipe that would be easy to scale up.
  • letsalcido, Thanks for the clarification!  Your putting forth the use of salt is making me think about it.  Glad you mentioned you used a solution.  Do you have a suggested range I might want to try or a suggested solution strength range?   I have been looking at posts here this afternoon and evening about liquid soap and found a post of mine regarding my procedure from 2016! 

    "Basically, my liquid soap is made by heating the oils, mixing the KOH with water in a plastic bucket until combined then adding the solution to the oils and stirring until saponified and it turns to a paste.  For me that takes about 10 minutes.  It is then covered and left overnight to make sure the saponification process is complete.  The next day the paste is weighed to determine the amount of H2O to be added, water is then heated then my thickener is added and stirred until dissolved, then the soap paste is added to the heated water and stirred then left to be dissolved by the heated water then covered. (glycerin can be added at this point if used).  Usually the by the next day the paste is totally dissolved and the fragrance can be added and it is weighed again to see if H2O needs to be added to bring it to the proper concentration reflected in the formula and it is then ready to bottle.  For this type of production a mixer is not needed."

    What concerns me is taking whatever I feel is right to correct this esthetic of my liquid soap and applying it to a large batch and being able to make it work!  I'm open for suggestions, my friend!

    David

  • @David08848 ; I just started making cosmetics/soap. I have a background in biochemistry but no industry experience. What I shared is what I have observed, experienced and found by doing some research online.

    I found a few sources, and this video has a great explanation for thickening soap with sodium. I believe she mentions that the maximum is 2% or you may break it (like I did by adding just a tad too much sodium) https://www.youtube.com/watch?v=y5z_zAnSEZg 

    It will be a matter or titrating until you reach the desired viscosity and documenting how much you used.
  • letsalcido,

    Just to recap, you showed two examples of your liquid soap in which you said on March 20th you used Polysorbate 20 to clarify them successfully and those are the pictures of the two green bottles that are above your comments about them?  The first one came out fine and to the second on you added salt which broke the emulsion.  On March 21st you said the two bottles of green you "fixed them separately with slightly different amounts of sodium".  So I am a bit confused.  Are you saying that the salt in small amounts can thicken a liquid soap and also give them some clarity and in larger amounts can either brake the emulsion and or cause clouding of the mixture?

    So does this mean that using salt in proper percentages can clarify and thicken a soap based liquid soap?  What about the Polysorbate 20?  Is that for clarification only or can that add to the thickening as well if not used in too high a percentage?  I just want to make sure I understand this before I go any further.  Thanks for your help!

    David

     


  • @David08848 ;

    The salt/sodium is specifically for thickening purposes. There’s a limit to how much you can use before it causes the soap to break/turn turn opaque.

    The polysorbate 20 is definitely needed for solubilizing your essential oils. The only essential oils I was able to use without it were peppermint and eucalyptus with menthol crystals (not sure if the menthol helps).

    I fixed two of my broken batches (not shown in any pictures) by diluting with castile soap 1:1 and adjusting the thickness with salt and coco betaine for each bottle. The pictures are the result of this. In the first picture I added slightly more salt to the half batch on the right, and it caused it to break.

  • @David08848 there is a blog post on this website that should help you figure out your salt curve.

    https://chemistscorner.com/why-does-salt-thicken-shampoos/
  • letsalico, Thanks for the clarification.  For the moment, I will stick with the PEG-150 Pentaerythrityl Tetrastearate because it has worked well and I still have a quantity of it to use up before I consider using salt but it is good to know the procedure!  I was planning on making a large batch then putting together very small containers to test with each scent I am considering using sort of like what is described in that link that alchemist01 posted from that Perry Romanowski guy!  (He looks so familiar!)  From my experience, I have found that fragrance oils can cause the same cloudiness as essential oils so if I can try each one with Polysorbate 20 in similar increments then record the results as suggested hopefully I can make sure that all scents have the correct percentages and give the best clarity possible!  Thanks, all of you!  I appreciate your help!  Looks like I'll be alone in my store over the next few weeks so that will give me the time to try all of this!
  • letsalcidoletsalcido Member
    edited April 2
    A few updates @David08848

    I ordered some PEG-40 Hydrogenated Castor Oil as it is supposed to be an even better solubilizer than Polysorbate 20.

    I also noticed that my soap is sensitive to temperature and gets very cloudy when cold. My uncle who has some experience with a shampoo he claims that Polysorbate 20 is cold sensitive, and solutions will turn cloudy. He had better success with PEG-40 HCO.

    I did a test and that was true, I put a clear solution at room temperature of E.O./Tween20 in water and it turned opaque. I doubled the concentration of Tween20 and it resisted cold temperatures but the amount I had to use was too high. 15% or so. I’m hoping PEG-40 HCO can be used at much lower concentrations for the same result

    Also, I didn’t know (newbie here) that liquid castile soap would turn very opaque (creamy) when cold. Is there a way to avoid this? Perhaps is the type of oils I used, and the solubility of the resulting soaps.
  • David08848David08848 Member
    edited April 3
    Luis, I really appreciate your input!  Your mention of PEG-40 Hydrogenated Castor Oil  rang a bell so I am starting to do some research and hopefully will find this available with one of the chemical companies here in New Jersey and New York so I can find a source and give it a try!  (I might even have a sample of it somewhere!  Also, I use Castor Oil in my formulation!)  

    I have found that in general liquid soaps can become cloudy on their own without a solubilizer when the temperature drops.  In my retail store here in New Jersey I have noticed differences in my liquid soap when the temperature starts rising in the Spring and lowering in the Fall.  They tend to stay clear in the Summer with a rise in temperature but I need them to be clear year round!
    It's helpful to hear your test experiences and with the small amount of experimentation I have had the time to do so far with the Polysorbate 20, I only have gotten small changes in the product. (and I wondered how much more I would have to add!)

    Without knowing the exact ingredients you are using in a liquid "Castile" soap it is hard to say.  This may have already been mentioned but liquid soap seems to perform the best when a zero percent superfat is used.  I did some research here and found a post about making liquid soap and the guy who was working on it said that he only used a 5% superfat and no one here picked up on it and mentioned that he might make out better with a zero superfat!  Sometimes, people see projects like these as being easy and "not rocket science" but this isn't always the case in my experience.  I have greatly appreciated your input and sharing, Luis!  Thank you!
  • So, as an update, I've been reading up on PEG-40 Hydrogenated Castor Oil and I went to the Protameen site, a local NJ company I've done business with for many years, and I see that they not only have PEG-40 but also 16, 25, 50 and 60!  I've only been looking up the 40 so I guess I can check with them and see what they suggest and do some research on the other options. I should have figured that it would come in various forms!  Life is a learning experience! :smile:
  • I saw that the PEG-40 Hydrogenated Castor Oil was "liquid to semi-solid" and the PEG-25 is listed as liquid so I'm getting the picture and I can see that most like the PEG-40 should be able to perform in the way that is needed... back to research!
  • Update:  I never heard back from the company which is not a surprise with the current situation we are going through but I did find an MSDS sheet that gave a range of 0.5%-5.0% as the suggested usage range.  I did find a couple of gallons of PEG-30 castor oil in my workroom but they weren't hydrogenated so that doesn't help.  Most chemical companies will give you a quote for a particular product but they don't list the price online and I doubt that I would hear back from them anyway right now!  The only other option might be a reseller but there were two examples I could find online.  One was 8.4 lbs. for $81.40 and the other was $110.00 for around the same size which sounds a little high to me.  Does anyone have a comparison price from a wholesaler they know for PEG-40 Hydrogenated Castor Oil?  That would be helpful!  David
  • David08848David08848 Member
    Update:  I finally heard back from my chemical company and they are sending me a sample of the PEG-40 Hydrogenated Castor Oil.  They asked about my procedure and pH range and I sent them this:

    "I saponify the oils until they become a paste and leave overnight.  The next day the dilution water is then added and the thickener and paste are added as well and are heated until the paste and thickener are dissolved and the batch is left to cool.  Then the fragrance, preservative and any percent of evaporated water are added and stirred until smooth." 

    Part of the concern they had is the pH of final product and it was suggested that:

    "I would start by mixing the fragrance into the Protachem HCO-40 and adding it to alkaline water roughly the same pH as your finished product.

    Traditionally you would mix the fragrance to the HCO-40, in a  10:1, 9:1, 8:1 etc.. Until you find the optimal ratio of HCO-40 to fragrance that will be soluble and clear in the water / surfactant.

    Every fragrance is different, so definitely test it out lab scale before production."

    I'm curious if anyone has any observations or recommendations about this!  Thank you!
    David

  • David08848David08848 Member


    Also, I didn’t know (newbie here) that liquid castile soap would turn very opaque (creamy) when cold. Is there a way to avoid this? Perhaps is the type of oils I used, and the solubility of the resulting soaps.
    letsalcido, I did find a brief article about castille soap that might offer a little information:


    Interestingly, since the temperature in my retail store has been in the low 70's F rather than 68 degrees F the top of the soap bottle have been a little more clear... Hopefully, the sample of PEG-40 Hydrogenated Castor Oil will arrive soon!


  • The PEG-40 Hydrogenated Castor Oil arrived the other day and I thought about how I should proceed and decided to try this:  I took a bottle of finished liquid soap was scented with Lemongrass Essential Oil at room temp. a few weeks ago.  I poured it into a glass measuring cup and added .4 oz. of the PEG-40 HCO.  I heated it up to about 120 degrees F and stirred.  It seemed to mix OK but I saw little "gels" throughout the mixture and did my best to stir as it cooled.  The temp dropped to about 100 degrees F and I poured it back into the container to see what happened.  Here is a pic with the new "gelled" batch on the left and the original batch on the right with the top 1" being cloudy (with a few air bubbles) the middle section being a little cloudy and the bottom 1" being clear!



    Here is the ingredients list posted before:

    Ingredients: 
    Water, Cocos Nucifera (Coconut) Oil, Oleic Acid, Ricinus Communis (Castor) Seed Oil, Potassium Hydroxide, PEG-150 Pentaerythrityl Tetrastearate, Glycerin, fragrance, Caprylyl Glycol, Phenoxyethanol, Hexylene Glycol

    Here is the procedure I use: "I saponify the oils until they become a paste and leave overnight.  The next day the dilution water is then added and the thickener and paste are added as well and are heated until the paste and thickener are dissolved and the batch is left to cool.  Then the fragrance, preservative and any percent of evaporated water are added and stirred until smooth."

    Here are my questions:

    A. Is using the PEG-40 HCO with the Crothix going to be a problem or has this occurred because of the order in which I used these in this attempt?

    B.  Should I add the fragrance and PEG-40 HCO together then add the Crothix to the batch after?

    Looking at it again - The sample is now 89 degrees and is evenly cloudy from top to bottom with no gel showing in it!

    Thanks for reading this and thanks for any assistance you can provide!
  • letsalcidoletsalcido Member
    edited May 11
    I hadn’t come to this places for a bit now.

    @David08848 I am trying hard to remember the name of that effect you saw in the soap. But it’s basically just telling you the PEG-40 HCO hasn’t mixed completely yet. You can see that effect when mixing glycerin into water.

    What’s interesting is that the bottle on the left is cloudier, and the only difference is the PEG-40 hydrogenated castor oil? Same amount of fragrance and temperature?

    I’ve slowly migrated to making a body wash not just with castile as there seems to be no way around the cloudiness. PEG-40 HCO has worked great at solubilizing my essential oils, making my gel absolutely clear. Given that your soap turned opaque later, I am thinking it must be a temperature issue. If it was due to the oils not being solubilized you would have seen the opacity change immediately after adding the oils.

    Maybe someone else has more ideas.

  • Luis, welcome back!

    I don't know the name either but it IS like what happens when you mix glycerin and water together!  To be clear in both pictures on the right are of an already  finished product from stock and nothing has been done to it and it's there just for comparison.  It shows the problem that was in so many of the liquid soaps I have made and it is there to compare it to the left one which is one of these that I have added PEG-40 Hydrogenated Castor Oil to, after it is heated, then it is stirred and then let sit for a while so we can see what it looks like.  Basically an attempt at "rescuing" some stock and making it usable if possible.

    In going back today, I see that things haven't changed and still look like the second picture of the liquid soap on the left.  When I pick up the container the liquid soap is still cloudy and toward the bottom of the bottle it appears to be gelatinous as well!  What I get from that is that I should have realized that the PEG-40 HCO needs to be in direct contact with the fragrance to work properly and then combined together and homogenized before adding them to the product.  (It can't hunt down bits of fragrance and work with each one of them!)

    So, what I am assuming is that it makes better sense to me to combine the PEG-40 HCO with the fragrance then add them to the liquid soap.  Once they are combined, I would then add the Crothix ( PEG-150 Pentaerythrityl Tetrastearate) to thicken it.  What I don't understand it what the one inch layer on top of the bottle consists of!  Is it a combination of fragrance and solidified soap?  I don't know.   But I do know that once I get this figured out, I can make some new liquid soap and hopefully have no problems with it which I am eager to do and can do during this difficult time while I work at my unopened store!  I am eager to find a solution!

    letsalsido, I posted a link to an article in a previous post for you that talks about liquid castile soap stating that clarity is an issue with this type of product!  Thanks again for your input!
    David 
  • Thank you, glad to be back!

    I think I remember the name of the effect, it’s the Tyndall effect if I’m not wrong.

    Yes they do recommend mixing your oils with PEG-40 HCO before incorporating into the product, but I’ve achieved completely clear gel washes by adding that or Tween 20 after I added the oils and it turned very opaque.

    I’m sure you can probably use less solubiliser if you mix the oils with it before hand. 

  • David08848David08848 Member
    edited May 12
    Ok, thanks.

    I will take a batch that is unscented but has been thickened with PEG-150 Pentaerythrityl Tetrastearate then combine a fragrance and the PEG-40 HCO together, heat and homogenize it then add it to the heated liquid soap, stir and let it cool down and see what happens!

    I am trying to figure out if PEG-40 Hydrogenated Castor Oil and PEG-150 Pentaerythrityl Tetrastearate together create a gel!

    More later!

    David
  • UPDATE!

    I mixed 0.4 oz. of PEG-40 HCO paste with 0.8 oz. Lavender EO and heated and stirred it until mixed.  I heated up 17 oz. of liquid soap stock I have that is thickened and unscented that I heated to 120F then added the fragrance to the liquid soap.  It came out clear!


    This was at 96 degrees!

    I went back a few minutes later and this is what I found:


    This was at 91 degrees and the bottle had begun to get cloudy!

    Yesterday, 20 hours later:



    Then the whole thing got cloudy!






  • David08848David08848 Member
    edited May 15
    Adding to the above posted earlier today...

    Last night I went into my large file for my Liquid Soap project and read through everything!  I usually try to collect as many formulations as possible but there weren't too many.  I did have a group of sources that mentioned that keep the superfat to 0% for this type of formulation to avoid clouding and I went in thinking that I should make sure that I had done it and I found the final formula with a note on it the there was a 2% superfat for the formula!

    So, this has got to be part of the problem and I will have to make a new batch to do my testing with 0% superfat in it!  Today I looked at yesterday's sample again to find that it had developed the same problem I had originally and that was clarity that is in the bottom portion and in this one is about 2" of cloudiness on top!


    In the upper left in the picture, you can see a very large white plastic storage bin in which the remainder of the thickened and unscented batch sits!  I will be making a new formula which I adjusted last evening and working off of that!  Nothing is easy!  Back to the drawing board but at least I can address the superfat issue!
  • BelassiBelassi Member
    I think your fundamental problem is the type of soap salts you have in there. For instance, a 30% potassium cocoate solution is a standard commercial item widely available. It is a clear low-viscosity liquid.
    The very first thing I would have done, is to carefully examine the profile of whatever oils you're saponifying and building a solubility table for each.
    It appears to me that what's happening to your soap is that one or more of the carboxylates is not very soluble and will only stay in solution at higher temperatures. I don't think the problem can be readily solved unless you move to a more precise formulation, that is, saponifying only pure, free fatty acids, eg oleic acid, (but you'd first have to check the solubility, I have no idea)
    Cosmetic Brand Creation. Concept to name to IMPI search to logo and brand registration. In-house graphic design inc. Pantone specs. Cosmetic label and box design & graphics.
  • Belassi, Hi there!

    As you can see here:

    Ingredients: Water, Cocos Nucifera (Coconut) Oil, Oleic Acid, Ricinus Communis (Castor) Seed Oil, Potassium Hydroxide, PEG-150 Pentaerythrityl Tetrastearate, Glycerin, fragrance, Caprylyl Glycol, Phenoxyethanol, Hexylene Glycol

    My first oil is Coconut Oil which is in the highest percentage, then Oleic Acid is next and Castor Oil is the last because it contains Ricinoleic Acid which makes a very water soluble soap and assists with lathering.  We're at about a 3/2/1 ratio for the three and in your post it appears that "postassium cocoate" and "potassium oleate" are good choices and as I mentioned Castor Oil makes a soap that is very water soluble!  I still wonder if the PEG-150 Pentaerythrityl Tetrastearate (Crothix) is part of the problem!

    Prior to the use of a solubilizer, my fragrances and essential oils worked fine at first but over time the clouding of the top 1" occurred and the unfortunate choice of superfatting the batch has to have played a part in all this!  I appreciate your input and I'll take a look at your suggestions.  Thanks!
    David




  • and as an addendum, I have a document from David Steinberg called "showletter" which I've had for years that contains several liquid soap formulas including "hand soap" "real soap shampoo" and all the formulas are made with fatty acids!...just sayin'
    David
  • BelassiBelassi Member
    edited May 15
    and all the formulas are made with fatty acids!
     - exactly. Not vegetable oils. 

    Cosmetic Brand Creation. Concept to name to IMPI search to logo and brand registration. In-house graphic design inc. Pantone specs. Cosmetic label and box design & graphics.
  • As I said above, Belassi

    My first oil in my formula is Coconut Oil which is in the highest percentage, then Oleic Acid is next and Castor Oil is the last because it contains Ricinoleic Acid which makes a very water soluble soap and assists with lathering.  We're at about a 3/2/1 ratio for the three and in your post it appears that "postassium cocoate" and "potassium oleate" are good choices and as I mentioned Castor Oil makes a soap that is very water soluble!  I still wonder if the PEG-150 Pentaerythrityl Tetrastearate (Crothix) is part of the problem!

    I spent the last hour trying to find a supplier for Coconut Fatty Acids which is much more difficult than I expected!  I saw listings that showed it to be a liquid and several pictures of liquids of various colors - golden to darker shades - and one from Acme-Hardesty for a 5 gallon pail  for $158.00 which was the only listing in the US!  The rest were from India and some listed it as "distilled"!

    If anyone has any US sources in the North East of the US, I would appreciate hearing about them!  Thanks!

    David

  • @David08848 I think you may be going down a rabbit hole here. Belassi is making some good points that may not be super clear. I’ll try ro expand:

    1) Fatty acids are not triglycerides, the first would be industrially refined and no longer attached to the glycerine backbone. So you would be able to buy high purity, reliable material. Some coconut and palm derived fatty acids: Stearic, Lauric, Capric and Caprylic Acids. This way you can avoid those that can’t solubilize at room temperature in their potassium salt form. However, if going this route you may be better off formulating a detergent-based wash. You can select for eco-cert options which are all naturally derived (but you’re already using PEGs so eco certification is out of the picture). If you decide to stick to true soap, you may need to live with the variability. Look at Dr. Bronner’s. They claim that their soap clouds at 70F, people may be ok with that. They’re also using basically all coconut oil. I threw a bottle in the fridge and it turned cloudy.

    2) The above means that by using vegetable oils you have a mostly unknown mixture of fatty acids (now carboxylates in water after saponification). Depending on the crops/harvest the oils may have different compositions so your results can vary from batch to batch. Kinda like wine, each vintage is different even if the bottle has the same name.

    3) Last but most importantly. Since the cloudiness seems related to temperature, I would be more inclined to think, like Belassi mentions, that it is some of the soap precipitating out of the solution. Do a test and dilute unscented soap 5:1, 4:1, 3:1 and add the solubilizer and oils (50g to 100g samples should suffice) . If they stay clear, it’s most likely the soap. The addition of the scent or the PEG-40 HCO is shifting down the solubility of at least one of the soaps, assuming the non scented version is completely clear at the same temperature. If you added the PEG-40 HCO and oil and it immediately turned cloudy, then it would be a matter of upping the solubiliser. Here it looks perfectly clear when warm. You also don’t need to warm your soap to add the scent and solubilizer mix. It basically emulsifies the oil into water, and emulsions are more stable at lower temperatures. Heating simply facilitates bond-breaking (increases solubility). In the case of liquid soap, heating promotes the release of the potassium ion from the carboxylates.

    I’m going out on a limb here but if adding the same amount of solubilizer without any of the fragrance also causes cloudiness it’s probably because there isn’t enough free water to bond to the soap molecules anymore, as other compounds are more readily hydrogen bonding. 

    This would be easy to fix, simply dilute your soap a bit more (5-10% more water maybe) and add more Crothix if you want to achieve the same consistency (it may not thin out too much). PEG-40 HCO is a foam enhancer so you may not see much change in foaming after dilution, as long as there isn’t excessive essential oil. 
  • Luis, I appreciate your input.  In my business I create handcrafted soap, liquid soap but I also make men's shaving cream and men's shaving soap which are made with fatty acids such as Stearic, Palmitic, Myristic and Oleic and I have done lots of research to learn about the fatty acid structure from low to high percentage to know exactly what to use to create the products I want and need including soap from the beginning of this project in 1998, but I don’t know everything.  My goal is to create products as simple as possible and as close to nature as possible but use ingredients that give the product the characteristics that the customers want.  I do wish to continue to make a soap-based liquid soap and I am willing to include ingredients that will create the best product possible even if some of them may not be considered natural.  If that means using Fatty Acids in a liquid soap formula, I am OK with that as I already use Oleic Acid as the middle of the three I have selected and I can also use coconut fatty acid in my shaving cream and my shaving soap so it would serve 3 purposes!  But I have already found that finding a supplier, or one that is willing to sell the quantities I need is not easy!  If[DP1]  it means I have to use a not completely natural solubilizer to create the best-looking product then I don’t have a problem with that either.

    Yes, I am aware of the differences in the various oils out there but I have been fortunate in my choices of suppliers and I have not found any raw materials that don’t behave the way that they should even though there may be slight differences from lot to lot.  Fatty Acids must meet the supplier’s requirements and be within the correct range and I believe they can create a much more consistent product than oils can.

    As far as the addition of PEG-40 Hydrogenated Castor Oil is concerned, it is a paste at room temperature and has the consistency of a “Vaseline” type substance.  The meltpoint of it is about 85-86 degrees F and my stock liquid soap has been around 70 degrees. I heated the PEG-40 HCO to around 100 degrees to be able to incorporate Lavender EO into it and I heated up the soap stock to around 100 degrees. After stirring the EO/solidifier together and adding it to the top of the liquid soap it sat on the top and had to slowly be stirred into the batch, which needed to be reheated a little, to get it to completely mix into it.  

    1. So, for me, I am still unsure what exactly is causing the problem but I am aware of one possible problem and that is that in my formula, I have a 2% “superfat”, yet in my research I have lots of sources that indicate the a 0% superfat is what should be used in a liquid soap because of the “clouding” that can occur if any superfatting is used!  So I will correct that issue!

    2.  I have recently heard that there are some “inconsistencies” in using “Crothix” PEG-150 Pentaerythrityl Tetrastearate as far as variations in results so I am looking into using PEG-150 Distearate.  I am still wondering if Crothix might be part of the problem.

    3.  It was also suggested that I might wish to try a blend of Polysorbate 20 and PEG-40 Hydrogenated Castor Oil

    4.  It was recommended that I might wish to try PEG-25 Hydrogenated Castor Oil which has a lower meltpoint so I will be giving that a try.

    5. My last concern is whether the size of my oil/soap phase might be too large at 24%/29.5% and this may be what you are referring to in your last suggestion in your mention of “free water” and adding a percentage of water that may aid if achieving a clear batch.

    As you pointed out, creating an “all natural” type of may not be easy and there are those who send out warnings about that temperature can change their product and that just goes along with the territory.  Also, testing the solubilizers without a fragrance might be a good idea as well and I had thought of that briefly but it stuck more in my head after you said that!  Right now, I’m happy to look at all aspects, then narrow it down and try, what I think are the right ones.  If I succeed then, great!  If not, I’ll know I did my best and that is all that matters to me!

    I appreciate your input, ideas and intelligence and am grateful that everyone here was willing to share their idea, thoughts and approaches!  Thank you one and all!  Thanks Luis!

    David










  • letsalcidoletsalcido Member
    edited May 20
    @David08848 it’s interesting that you mention your PEG-40 Hydrogenated Castor Oil is a paste. I would double check with your supplier because it may actually be PEG-20 Hydrogenated Castor Oil which is a paste at room temperature for what I have seen.

    I did find online a brand that was selling a 2.2lbs bucket of PEG-40 Hydrogenated Castor oil (main label) but when I read the INCI name in the back it said it was the PEG-20 version. For what I have seen (and what I have with me) PEG-40 will be an off-white or yellow honey-like liquid (not as crystal clear, but translucent), theirs was a paste.

    Either way, both should work as solubilizers, just the PEG-20 would be less soluble in water and probably have a different efficiency. 

    Polysorbate 20 works great too, not sure if it’s necessary to mix. But I did notice with a formulation I was making that adding polysorbate 20 thinned out my gel a bit.

    For thickness you could try PEG-120 Methyl Glucose Dioleate (sold by Lotion Crafter, Making Cosmetics, and others as some name with the suffix DOE, it’s a 10% active solution with 10% Methyl Gluceth-10 (humectant)). This is a liquid and easier to work with than PEG-150 Distearate which requires heating and in my experience took a bit to dissolve. Also some people here claimed it can make your formulation susceptible to temperature, turning like jelly at cold temperatures and water thin when warmer. I made a serum with it, threw it in the fridge and I didn’t observe any gelling, but your mileage may vary.
  • Luis,  a quick question!  What temperature is it in the room that you saw, worked with or touched the PEG-40 Hydrogenated Castor Oil?

    My workroom is between 68 and 72 degrees Fahrenheit!  Many of the online pictures I have seen of PEG-40 Hydrogenated Castor Oil show it as a white paste!  I just checked back at my email and PEG-20 Hydrogenated Castor Oil and it is described as "a clear liquid at Room Temp and a little below" which makes more sense to me since it would have a lower viscosity?

    David
  • letsalcidoletsalcido Member
    edited May 20
    @David08848 let’s see if other people here have knowledge of which one is the correct one. My room is also around 70. 


  • The ebay one lists itself as "Ethoxylated" as does the ulprospector one but the other two don't.

    https://www.wisegeek.com/what-is-ethoxylation.htm
  • @David08848 yes, even though not all listings mention it’s ethoxylated, the fact that it’s a PEG compound means they all are.

    I hope you can figure out what’s causing the cloudiness with your soap!
  • David08848David08848 Member
    edited May 20
    Let me make it simple:  
    1.  Formula had a 2% superfat instead of recommended 0%
    2.  Crothix may be the problem - perhaps use PEG-150 Distearate
    3. trying of a blend of Polysorbate 20 and PEG-40 Hydrogenated Castor Oil might be an option
    4.  try PEG-25 Hydrogenated Castor Oil which has a lower meltpoint
    5. the size of my oil/soap phase might be too large at 24%/29.5%

    Comments?
    Thx, D


  • My opinion on those:

    1. The cloudiness due to superfatting probably would have been apparent even before adding the solubilizer, but may as well try 0% superfat.
    2. Consider PEG-120 Methyl Glucose Dioleate instead of PEG-150 Distearate as is easier to work with and also a good thickener.
    3. Could try Polysorbate 20 alone too. That and PEG-40 HCO are benchmark solubilizers. You’ll notice that more moles of ethylene oxide on an oil makes them more water soluble.
    4. PEG-25 HCO may have a lower melting temperature but won’t behave the same way. I suspect it’s used more often to emulsify heavier oils. Here’s a good reference I found https://www.ulprospector.com/documents/1599881.pdf?bs=29781&b=1462555&st=1&sl=90656870&crit=UEVHLTI1IEh5ZHJvZ2VuYXRlZCBDYXN0b3IgT2ls&r=na&ind=personalcare doesn’t hurt to try.
    5. Your soap should be less than your oils because of the glycerine produced. But yes, diluting a bit further would be good to try. Maybe 1:4 saponified oil to water instead of 1:3.
  • David08848David08848 Member
    edited May 20
    Luis, thanks for getting back to me on these.  
    1. Recalculated SAP values for formula last night - it is actually a 4% superfat!  (rolls eyes :(  )  have changed formula to 0% superfat.
    2.  Did find a reseller for PEG-120 Methyl Glucose Dioleate version: PEG-120 Methyl Glucose Trioleate (and) Propylene Glycol (and) Water - 4 lbs = $125!   :o - still looking...
    3. I have to take care of superfat first then go onto trying PEG-40 HCO again. 
    4.  PEG-25 HCO and maybe blends of this and the other two but I have to check out the information and decide where to go with this.
    5.  In soapmaking arenas an "oil phase" IS the percentage of the oils in the formula but a "soap phase" is the amount of oils and the amount of hydroxides together... just different terminology and a different approach.

    In the soapmaking "arena" liquid soaps are made with a larger percentage of water and "cooked" (cringe! :s ) for at least 3 hours until it goes through several "phases".  I don't use that approach and it takes me about 10 minutes using about a 66% of water to process the 33% of oils + lye then it is left overnight to finish saponification.  The actually oil percentage in the finished formula is 24% and the water phase includes water and glycerin at a little bit over 60%.

    Since two fragrances, Musk and Rose do not show this problem at all, points a finger toward fragrance as being a major part of the issue but I think the "unsaponfied oils floating around" because of the superfatting are "interacting" in some way with the rest of the essential oils/fragrances oil making it easier for this problem to occur so I need to take care of the superfat first!  A bucket of Oleic Acid arrived yesterday so I can get going on this soon then move onto the next step!  My only other concern is the ratio of oils and at a 3/2/1 ratio of Coconut /Oleic/Castor may need to be looked at but I do have several old formulas with just Coconut oil in them or combos with Coconut Oil being the higher percentage over other oils such as Oleic Acid and Soy.  Anyway, I would rather go into something with as much knowledge as possible and having done as much research as possible!  You gotta know all the players!  Thanks, Luis and everyone!

    David
  • Cafe33Cafe33 Member
    edited May 31
    Hi David, I wanted to share that there is a distributor here in Mexico for Coconut Fatty Acid, and it is 4.73 USD per Kg (with a MOQ of 1 kg). I know it is late in the conversation but I am following your thread.  
  • David08848David08848 Member
    edited June 1
    Hi! Thanks for following and sharing! If I did the calculations correctly, that would be about $2.15/lb. for the Coconut Fatty Acid with a minimum of 2.2 lbs. purchase. but coming from Mexico what would the shipping costs be?

    I heard back from deWolf in Rhode Island (near where I grew up) and they have a minimum of a 55 gallon drum and others I contacted didn't reply! What company in Mexico would this be so I could check it out?

    I redid the formula for the liquid soap and made sure there was no superfat included in it this time! During this difficult time, I thought it was a good idea to work on all reformulation projects, completed the Shaving Cream final formulation a few weeks ago, the liquid soap formula last week and yesterday the Shaving Soap formulation so I will be trying all three soon and trying the PEG-25 Hydrogenated Castor Oil sample I received last week with one of the sample batches and see how it goes with the new liquid soap formulation. Thanks for your input, Cafe33! David - Everyone, please stay well!
  • Cafe33Cafe33 Member
    I wanted to share the price info with you (I think you had mentioned 168 USD for 5 gallons?!) I do not know if they will ship to the USA.

    Also, 4.73 USD was the price for 1 kg pack size. I have not inquired on larger pack sizes but from my experience, they can go down by 20% or so even purchasing as little as 5-10kg. 

    Either way, I have sent you the complete info by private message. 

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