creams separating - Chemists Corner

Formulating

creams separating

Posted by rosa on August 20, 2015 at 10:00 pm

I have had problems lately with creams separating I am trying to narrow down what could be the problem.

Basically, I have an oil in water emulsion (18% oil phase); 6% is emulsifier, 3% butter etc. and various oils.

Water phase contains MSM, GABA, pro vit B5, hyaluronic acid, niacinamide, hydrolysed proteins (cationic) (1%), beta-glucan (0.5%), etc.

My suspicion is cationic hydrolysed proteins or beta glucan?

Separation seems to happen regardless of emulsifier; I used BTMS which is also cationic so thought it would give me trouble but when switched to Olivemulse (Olivem1000) same thing happened - first breaking/curdling a minute or two after combining the two phases at 75 degrees celsius, then emulsification..which later separates (layer of oil on top and thinning of cream) after potting.

The cream was holding up better when I used cocoa butter, but appeared more prone to separation when I switched to avocado butter as I thought the cream was too stiff, so unsure if this made it weaker (less viscosity)?

Any help with this would be greatly appreciated as really tired of it by now!

Rosa

johnb replied 7 years, 8 months ago 9 Members · 25 Replies
25 Replies

David

Member
August 20, 2015 at 10:58 pm

1. calculate the HLB

2. choose the correct emulsifier

3. Make a sample without “MSM, GABA, pro vit B5, hyaluronic acid, niacinamide, hydrolysed proteins (cationic) (1%), beta-glucan (0.5%), etc. ” -it should now be stable

4. Add a preservative

5. Add the ingredients from point 3 one by one and take notes.
MarkBroussard

Member
August 21, 2015 at 3:47 pm

@rosa:

Are you homogenizing continuously from the time you add the two phases? Regardless of the ingredients, if you do not homogenize until your emulsion reaches 50C or below, you will get separation.

I ask because your statement “ first breaking/curdling a minute or two after combining the two phases at 75 degrees celsius, then emulsification..which later separates (layer of oil on top and thinning of cream) after potting” … makes me think that perhaps it’s a technique issue and not an ingredient issue.
rosa

Member
August 21, 2015 at 4:27 pm

Hi, yes I do stir continuously down to 40-45 degrees. At ~50 degrees the creams is really thick, so thick/viscous so it is impossible to stir with emulsifier. Instead I have to use a hand whisk. And later on (usually when adding additives around 40 degrees), a bit of thinning occur (not a huge amount). Then for some reason, it becomes thinner/unstable.

What is really happening with the cream. Could it still be a technique issue?

I do realize I have to do test batches and eliminate one by one ingredients, but really want to narrow it down a bit first!

Thanks a lot for the help David and MarkBroussard
MarkBroussard

Member
August 21, 2015 at 5:12 pm

@rosa:

Looking at your ingredients, I don’t see any there that should be problematic.

If you’re using Olivem, you’re going to want also add 2% Glyceryl Stearate, 1% Cetyl Alcohol and 0.2% Xanthan Gum to stabilize and thicken the emulsion. I would try that first.
rosa

Member
August 21, 2015 at 5:46 pm

I have heard that xanthan gum does not go with BTMS as both are cationic, is this true?

I also thought olivem is a strong stand-alone emulsifier? So it really need co-stabilizers?

I never used glyceryl stearate, but is seems to be a good product?

The fact that the cream curdles immediately when combining the phases, doesn’t that really mean that something doesn’t really go together in there?

Thanks a lot!

Rosa
Microformulation

Member
August 21, 2015 at 5:51 pm

All the info about Olivemulse is available on the vendors page. It answers almost every one of your question; http://www.ingredientstodiefor.com/item.php?item_id=1223

Also Olivem 1000 is very process dependent. I wouldn’t try making it with a whisk or any less sophisticated mixing equipment. I have to agree I think it is linked to your technique and available equipment.
MarkBroussard

Member
August 21, 2015 at 6:06 pm

@rosa:

Yes, that “self emulsifier” line is marketing schtick. The only way you’re going to get a stable emulsion with Olivem 1000 is as I described. I use it extensively and this is how you get a stable emulsion with it.

I do not use BTMS so can’t offer you any advice there.

Are you using a homogenizer or some other piece of equipment? It really does need the power of a homogenizer to get a stable emulsion.

Hope that helps.
rosa

Member
August 21, 2015 at 6:49 pm

I am using an emulsifier (cheaper version of a Silverson type), but as it goes thick really quick when cooling (5-7 mins) I am not able to stir much longer, but have to continue hand whisking…could that be the problem?

Would those extra ingredients likely stabilise BTMS as well? When using BTMS, I usually use a combination of BTMS and E-wax, i.e. 4% BTMS and 2% E-wax, which I have seen other people do..

Thanks!

/Rosa
Microformulation

Member
August 21, 2015 at 7:32 pm

BTMS is a whole different animal and in my experience used mainly by Crafters at least now for the most part. For more info on BTMS I would refer to Croda.

Xanthan gum can stabilize a Formula by increasing the viscosity of the continuous phase. However as Mark pointed out your failures are immediate, not over time.

You have some very general questions so (no offense) I think some reading and research on emulsification and emulsifiers could be in order.
Bobzchemist

Member
August 21, 2015 at 10:22 pm

I hope I’m not sounding like too much of a broken record about this, but I think you should try two approaches.

Firstly, drop the Olivemulse (Olivem1000) and the BTMS completely. Make your emulsion with one of the more fool proof emulsifiers, like Pemulen TR-1 or TR-2 (depending on how much oil you use)

http://www.personalformulator.com/wvss/product_info.php?products_id=1010 

Secondly, make an Olivem or BTMS emulsion but drop out everything but water, emulsifier and oil phase.

Let us know how this all turns out.

As far as equipment goes, I think you should seriously consider either a decent overhead mixer or a heavy-duty kitchen stand mixer. Using a whisk is probably the worst thing you could do to an emulsion.
MarkBroussard

Member
August 21, 2015 at 11:50 pm

@rosa:

I would try cutting down on the oil phase + butters to no more than 15%. I have found that Olivem will not form stable emulsions with oil content much above 15%.

Another question: Are you using Hyaluronic Acid (SLMW) or a higher molecular weight HA?

When you say “Water phase contains MSM, GABA, pro vit B5, hyaluronic acid, niacinamide, hydrolysed proteins (cationic) (1%), beta-glucan (0.5%), etc.” … Are you adding these ingredients to the water phase prior to forming the emulsion? If so, that may be your problem. Try first forming the emulsion and then adding these ingredients, one-by-one, at 40C or less.
rosa

Member
August 22, 2015 at 8:13 pm

Most of these are going into the water phase heated, except hydrolyzed proteins. How should I add them, dissolved in small bit of water? Not as powder I suppose? Why is that better? I do need quite a lot of water to dissolve in..

I suppose that would be a way to see if any specific ingredient is causing problems, but I have no idea how to add those ingredients after?

I am using the low molecular weight HA, is that ok? What is the difference from a formulating point of view?

I know I have a lot to read and I have made creams some time, but it has been stable lately, so very surprised the separation issue starts again!

And I am very happy for all the help!

Rosa
MarkBroussard

Member
August 23, 2015 at 2:20 am

@rosa:

Olivem 1000 is a finicky emulsifier and forms a lamellar structure, so lots of ingredients in the aqueous phase pre-emulsification can have a negative effect on forming a stable emulsion.

Yep, you can just add your ingredients as powders directly to the emulsion under high shear … they will dissolve/disperse in the emulsion with homogenization. Or, if you want to hold back some of the water and dissolve the solid ingredients in a small volume of heated water, no problem.

SLMW HA will not form a gel. Higher MW HA will gel and thicken your aqueous phase and may have an effect on the emulsion.

So, to sum it up … Olivem 1000 does not form stable emulsion solo … you need to also add Glyceryl Stearate, Cetyl Alcohol and Xanthan Gum. If using Olivem 1000, you should minimize the ingredients in your aqueous phase pre-emulsification and add them post-emulsification at cool down. Olivem 1000 does not form stable emulsions if the oil phase is much above 15%.
rosa

Member
August 23, 2015 at 10:57 am

Thank you so much - I will try this and see how I get on.

How long is usually necessary to homogenise/emulsify to form stable emulsion as I think the fact that with some creams, likr the one separation, I am not able to stir more than 5-7 mins..that really is too short? What I cannot understand is why it goes really viscous so quich, just to turn runny after?

Another question; A friend of mine is in the food industry and gave me some samples of food emulsifiers, i.e sucrose esters (Sucrosilk SP10) or Sucrose Ester SP50..anyone heard of this before being used in cosmetics/creams?

Thanks again!

Rosa
belassi

Member
August 23, 2015 at 2:18 pm

Get some SP70 and try it.
rosa

Member
August 24, 2015 at 8:23 pm

Thanks a lot for all the help..have ordered ingredients and with make trials once they arrive!

What is the difference between the different numbers (SP10, 50 or 70), Belassi?

Rosa
belassi

Member
August 24, 2015 at 9:30 pm

According to the published information it’s like a number line with the ones on the left for o/w and the ones on the right for w/o.
rosa

Member
August 25, 2015 at 7:46 pm

Oh..thanks! I didn’t have any idea!

Rosa
Chemist77

Member
August 26, 2015 at 10:10 am

http://www.in-cosmetics.com/__novadocuments/34394?v=635115553049200000

here you go @rosa
rosa

Member
September 2, 2015 at 6:24 pm

Thank you so much!

Rosa
rosa

Member
September 4, 2015 at 4:55 pm

I will try the formulation with OliveMulse with added glyceryl stearate (2%), cetyl alcohol (1%) and xanthan gum (0.2%)..so a bit excited!

I presume this means I should reduce hard wax/butters by the extra 3% glyceryl stearate and cetyl alcohol?

Also, should I leave out the xantan gum along with all the other ingredients until stable emulsion is formed? And then add in one by one of the ingredients?

Thanks for all help!

Rosa
rosa

Member
September 7, 2015 at 7:50 pm

I made the cream like MarkBroussard advice and it turned out looking really different and very stable and I am really grateful for this Mark! Thanks a lot for the advice all of you, but this specific advice was really suited to my cream

Really appreciate it!

Rosa
MarkBroussard

Member
September 7, 2015 at 8:25 pm

@Rosa:

My pleasure. Glad to hear that you had some success!
Zink

Member
March 31, 2017 at 1:53 am

Digging this one up.

I just tried to use BTMS for the first time, all was fine until I added DL Panthenol in the cooldown phase; instant curdle. Perhaps it holds negative charge.
johnb

Member
March 31, 2017 at 6:56 am

Zink, be aware that panthenol is not the inert, benign material that is is often assumed to be. If you look more into its constitution you will see that it is a derivative of propanolamine: N-Pantoylpropanolamine