# Same batches - but some bottle separating



## PrairieLights (Oct 25, 2014)

Help, scientists and chemists! I had separating occurring on parts of the SAME batches of LS, so I broke it all down and tested individual ingredients. All fine. Recombined and now some are doing it again! Same recipe, same batch... and yet....
Help?
On an interesting note - I made a batch of shampoo for the fun of it and ONE bottle turned almost solid! The other 3 bottles did not! What in the world?!?!?! But those are for personal use, so no biggy. The LS issue - now THAT I need some insight on. 
TIA *hugs*


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## Susie (Oct 25, 2014)

OK, we're going to have to know the recipe(s) and what EOs/FOs were used in what.  Because this is probably going to come down to the EOs/FOs, but maybe not.


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## PrairieLights (Oct 25, 2014)

But why, if it is either, would part be fine and part not? Litsea in one is clear - Litsea in the other is not. Same recipe. Another is euc and spearmint... fine in one, not in the other jar. Ack. I cannot see the pics I posted to say more... other than my newest batch - I used fragrance oils instead. Lavender vanilla, .... oakmoss and amber.....:think:.... and vanilla. 
My secret recipe? Would that make a difference from bottle to bottle? My husband said "It's like they don't like the larger bottles!"  It is 33% coconut, 5% avocado, 7% castor, and 55% olive. 5% SF. 

And the whole shampoo thing - now is that weird or what?!?! I am voting that it is an altitude issue. Yes, my bathroom must be higher up than my son's bathroom. 

Thank you for putting your thinking cap on with me!!! <3


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## Susie (Oct 25, 2014)

OK, first thing that jumps out at me is the 5% superfat.  I have never had a batch with higher than 3% that did not separate.  And I have had issues with 3% separate if I used any citrusy EO whatsoever.  I don't exactly know why, but I am sure someone here does.  I just know that if I am using citrusy EOs, I need to keep the superfat at 2% or lower.  I have never used FOs, so I can't help you there.  

If you separated the paste out into separate jars for dilution, I would guess that you scooped out the top into certain jars, then the bottom into others.  The more superfatted top portion would yield more separation than the bottom.  If you diluted all of the paste at once, I have no idea.

Now, as to what to do about it...ask IrishLass, DeeAnna, or FGOriold.  They are our sciencey soap gurus and can tell you all about polysorbate.  If you happen to have some, I think(you need to wait to hear from them to be sure!) you warm up the soap and add a bit at the time until it all goes back together.  *Here is the post where IrishLass talks about adding polysorbate 80 to clear up an FO/EO issue:

http://www.soapmakingforum.com/showthread.php?t=48465

If you don't have any, you can mix a bit of KOH with water to add a bit at the time to lower your superfat.  Let me see if I can go find those posts for you.  I will edit this then.  (I stole a line I copied from DeeAnna's how to fix broken soap post.)

*First, put 0.4 oz KOH in 2 oz water. Mix until dissolved. Measure 1 TBL of this solution into your soap. Stir. See what happens. If needed, add another 1 TBL, and see what happens.*


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## PrairieLights (Oct 25, 2014)

I diluted all of it at the same time...
So some of the 5% SF is fine - no probs - but you think perhaps adding the fragrances caused problems with the SF? I am nervous about adding any more KOH just because one jar separated and one didn't... but I might try that. I am jotting your notes down, stolen or not. LOL. Thank you Susie! I appreciate your help trying to figure this out. :crazy:


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## DeeAnna (Oct 25, 2014)

Yanno, it's really hard to troubleshoot problems like this because we're not watching right over your shoulder as you do your dilutions and fragrancing. What may seem like an insignificant thing to you might be a big deal to Susie or the rest of us. Frustrating, isn't it! 

Okay, so Susie is saying 5% SF in liquid soap is a big deal. I gave that a think, and came up with an explanation that may be helpful to you --

Let's say you use a large container to dilute enough paste to make a total of 2 quarts of diluted soap. After diluting and fragrancing, you pour this large batch of LS into 2 separate quart jars. Let's also say that the 5% SF or the fragrance or both has caused the diluted soap to have some free fats and/or free fatty acids floating around. At the point when you pour the soap into the two jars, however, the diluted soap will look perfectly fine because you just got done stirring it and it has not set quietly for very long.

That said, there may be enough invisible separation occurring so the first jar has somewhat (or a lot) more of the free fats and fatty acids and the second jar contains less -- maybe a lot less. Let the two jars sit for awhile so the fats or fatty acids can rise to the top of the liquid. Voila, you'll see a lot of separation in one jar and less or none in the second.

I'd recommend you follow Susie's suggestion about fixing it by adding some KOH to the separated soap. Keep track of how much KOH solution you use per, say, 1000 g of diluted soap or 1000 g of the white separated stuff. If the separation is fatty acids or fats, you should see the white top layer gradually disappear as the KOH turns the fats or fatty acids in that top layer back into soap. 

Remember, you can do this to just one container and see what works. You don't have to mess with all of the soap all at one time. If this does fix the separation, you can use the amount of KOH needed for the one jar to help you fix the others.


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## Susie (Oct 26, 2014)

^What DeeAnna said!

Yes, what I am trying(and failing) to convey is that even though the paste and diluted soap *looks* identical, you get higher amounts of fat in one portion compared to the next.  I have had it happen more than once.  Even on my 0% superfat laundry soap, I have to be sure to get all of the paste from top to bottom from one area rather than scooping off the top to prevent getting some separation once I add the EOs.  

Please note that this happens MUCH more often in larger batches for me.  I seem to do fine in 16 oz oil recipes.  But larger than that, it gets dicey.


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## PrairieLights (Oct 27, 2014)

Thank you, both! I am going to go ahead and give the KOH a try on one and see what happens. In the meantime, I am thinking of only making unscented soap, then warming up and fragrancing prn. It seems when I have done this in the past for just the fam, it didn't have probs. Did adding germall plus contribute to my sep? It is also my first time using that yucky stuff...... oops, I used an adjective. I mean, it is the first time using that. 
Thank you thank you thank you!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!  You gals are WONDERFUL! <3


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## DeeAnna (Oct 27, 2014)

I haven't had any problems using germall plus in my diluted soap. That isn't a definitive answer, I know, but I wouldn't expect this stuff to cause problems. I've had more experience with my EOs clouding my diluted soap. Germall plus seems to be a pretty good player in the products I've used it in (lotions, diluted LS).

I really think Susie's concern about your superfat is the direction I'd look at first. This is an issue that comes up a lot when people are having trouble with LS.


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## PrairieLights (Oct 29, 2014)

Follow-up: The fragrance oil batches are now back to how they were - about 1" top layer of yellowish goo. I will try one more tablespoon today and if that doesn't work, I suppose I throw it out and never use those f/o's again.
So y'all don't superfat your liquid soap? But people love how moisturized their skin feels after using it....... I don't want to change it and disappoint...


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## Susie (Oct 29, 2014)

I use no more than 3% superfat.  And no more than 2% if using citrus EOs.


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## seven (Oct 29, 2014)

what Susie said regarding superfat. no more than 3% for me too. i usually go with 2% max.


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## Spice (Oct 30, 2014)

I had read a post in another forum that castor oil was very picky when SF. The recommended SF with castor oil was something like 1%.


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## Susie (Oct 30, 2014)

I usually have castor oil at the 5% range in all my hand soaps.  Not usually in my laundry soap because I have an HE machine, and I do not need the bubble monster.  I have never had any problem with that.  It is just the superfat that causes problems in my experience.  YMMV


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## PrairieLights (Nov 4, 2014)

I have not had many issues with the essential oils overall - but the fragrance oils I used this time - BIG problem! I ended up throwing them out. I added the KOH and they stayed the same - but the pH soared to over 20! (It broke my meter!) I think I will bring my recipe down to 2-3%, per your recommendations, and see if I can keep this from happening again... BUT I don't even want to try fragrance oils now! I appreciate all of you! I really do! :-D


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## DeeAnna (Nov 4, 2014)

"...the pH soared to over 20! (It broke my meter!)..."

By definition, pH can only go to a high of 14. If the meter showed 20, it was broke, no doubt about it, but it wasn't from the essential or fragrance oil you were adding. You are assuming your meter going haywire was a consequence of adding the fragrance, but I'd say the meter ... just broke. 

It's a little like the situation when a car quits right at the moment the driver was changing the volume on the radio. Changing the volume and the engine quitting at the same time was just a coincidence. The real reason was the car ran out of gas.


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## Susie (Nov 4, 2014)

I hope you can still get those FOs out of the trash!  It is not the FO that caused the pH change.


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## PrairieLights (Nov 10, 2014)

I pulled out the pH paper and used it - it turned BLACK. 
What was the problem, then? Remembering the same batch of unscented and essential oils are fine... It was VERY sad to pour it out. Not only because money is an issue - but because the vanilla looked and smelled like caramel - the best vanilla LS I have ever smelled or looked at! So sad. So so sad.

A few days ago I tried a lower SF and that different dilution method... and it is cloudy. GAH!!! I usually like trying new things... :roll:  At least I have several batches of EO and unscented that are good to go.  I do love learning though - so school me!!!


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## Susie (Nov 12, 2014)

PrairieLights said:


> I pulled out the pH paper and used it - it turned BLACK.
> What was the problem, then? Remembering the same batch of unscented and essential oils are fine... It was VERY sad to pour it out. Not only because money is an issue - but because the vanilla looked and smelled like caramel - the best vanilla LS I have ever smelled or looked at! So sad. So so sad.
> 
> A few days ago I tried a lower SF and that different dilution method... and it is cloudy. GAH!!! I usually like trying new things... :roll:  At least I have several batches of EO and unscented that are good to go.  I do love learning though - so school me!!!



Well, I need to know your SF and dilution method before I can help you.  Also, did you use a lye calculator, and if so, which one.  Just take us through what you did from start to finish.  Also,  I have never used pH paper to measure soap pH, so black means nothing to me.  I need definition on that one.


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## sapuncic (Nov 28, 2014)

:?Dear Soapers this is my first post on the forum even though I have been reading it for the last couple of years since I started soaping. Just to say that the forum is full of great and useful info and I would like to thank everybody for sharing their experiences as it helps a lot! :smile:

I've decided to post in this thread since I am experiencing similar problems with my 100% Olive LS batch, and I am hoping that somebody has words of wisdom for the two issues below.

I have made a batch of Castile LS with 1:2 water to glycerin. The recipe used is:
500g Olive oil 
100g KOH
104g Water
200g Glycerin

After cooking it for 3-4 hours on the stove and in the oven, I let it sit covered with a blanket until morning. Then I scooped the paste randomly into 2 different pots for dilution. 
First was diluted to have 20% actives in the soap. (100 g paste + 266 g dilution water having in mind the water that evaporated during cooking).
Second was diluted with more water (100 g paste + 400 g water)

The first problem is that the more diluted one separated (second photo) and the one @20% actives did not (first photo, first jar from the right). Any ideas on what might have happened here?







The second problem is with the FO (first photo, first jar from the left). I've used BB Blueberry Delight FO. I took 120 g of diluted soap and aded: 3 g FO + 0.2 g vitE oil + 3.2 g polysorbate80. 
Now the brown color is probably from vanilla present in the FO (FO has 8% vanilla), but what I don't get is why it is on the top since I've added PS80??? :???: maybe I should add more PS80...any thoughts on this?

Just for info, the middle jar is colored with BB Cherry Blossom FO. It has slightly lighter color then the non-scented one but has no separation so it looks fine to me. I don't care much if it is transparent or no as long as it cleans and bubbles.

Thank you in advance for any advice you might have!!! :wave:


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## Susie (Nov 28, 2014)

Too high of a superfat.  Best as I can figure, you had somewhere in the 4.5% superfat range.  Superfat will always gather in the top portion of paste.  So when you go to use a paste that has sat a while, the higher superfat is in the top portion.  Don't ask me how that happens in that thick of a paste, but every batch of paste I have let sit for a while with any superfat higher than 3%, it always happens.

If I am going to let paste sit for a while before dilution, I will usually go ahead and divide it while it is still very warm to the touch.  This helps keep this from happening for me.  

I am pretty sure the polysorbate 80 should have helped with the separation, but I have never used it, so I am going to have to let more experienced folks help you there.


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## sapuncic (Nov 28, 2014)

Thank you Susie for the reply as well as for the tip for the paste!  Next time I will do as per your advice or  if I let it sit longer then I will mix the paste thoroughly before dividing for dilution.
Although I am pretty sure I randomly scooped the paste out (top and bottom and around the pot). 
I was afraid it might be the superfat, although I intended to have 0% superfat. The thing is that Summerbee calc was giving 101.7 g KOH for 500 g of OO & 0% superfat, but my KOH vendor told me that the KOH purity is 95% and so I reduced KOH to 100 g since summerbee calculates for 90% KOH purity.
Seems like my KOH might be closer to 90% and not 95% as I was told :-x


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## Susie (Nov 28, 2014)

Yeah, I never change the amount of KOH(or NaOH) that the calculators tell me to use based on what I think or the vendor thinks the purity percentage is.  I have yet to have any problems related to KOH purity.


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## sapuncic (Dec 8, 2014)

Yeah...I will not do it again definitely. Thanks for sharing your experience! :smile:

I am not sure what to do with the one that separated....to discard the top layer and use the rest or to add some Polysorbate80.... or maybe add some dissolved KOH, cook a bit and see what would happen... :?:


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## sapuncic (Dec 8, 2014)

I did some heavy thinking these days regarding soap separation....

Is it possible that in the case of superfated soap a more diluted soap would be more likely to separate since there will be an increased difference in viscosity/density between soap (bottom layer) and oil portion (top layer), compared to less diluted one where soap and oil portion might have close densities and therefore oil portion stays suspended in the soap... :?:

Any thoughts on this theory?


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## Susie (Dec 8, 2014)

I have not had the years of experience making liquid soap that some of these folks have, so I may not be the best person to give an opinion here.  Hopefully, a few of them will step in and answer that.

My experience has been that three things cause separation only:  Too high superfat, certain oils, some FO/EOs.  I am highly diluting liquid soaps for foamer bottles, and have had no problem with separation.  

My theory on the oils that cause separation are that the extraction methods might be different or someone has added other oils to them.  They seem to be inconsistent on whether they cause separation or not.  I have become extra careful to note the brand of oil on every recipe.  That way if I have problems, I can easily see if it is tracked to one manufacturer or not.  I may never use all this information, but better to have it and not need it than need it and not have it.(I need to get all of this on computer so searching it will be easier!)


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## FGOriold (Dec 8, 2014)

sapuncic said:


> I did some heavy thinking these days regarding soap separation....
> 
> Is it possible that in the case of superfated soap a more diluted soap would be more likely to separate since there will be an increased difference in viscosity/density between soap (bottom layer) and oil portion (top layer), compared to less diluted one where soap and oil portion might have close densities and therefore oil portion stays suspended in the soap... :?:
> 
> Any thoughts on this theory?




Here is an interesting read on that subject that might be helpful. It is more about gravity than density though:

http://swiftcraftymonkey.blogspot.com/2014/12/weekday-wonderings-using-polysorbates.html


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## DeeAnna (Dec 9, 2014)

Specific gravity is basically density of any material divided by the density of a "reference" material. Usually the reference material is water. Here are two examples of the same oil and how you would end up with the same specific gravity number from density in two different kinds of units (grams/milliliter and pounds/cubic foot):

Water density = 1 g / mL
Oil density = 0.92 g / mL

Specific gravity of oil = Oil density / Water density = 0.92 / 1 = 0.92

Water density = 62.4 lb / cubic foot
Oil density = 57.41 lb / cubic foot

Specific gravity of oil = Oil density / Water density = 57.41 / 62.4 = 0.92

***

"...Is it possible that in the case of superfated soap a more diluted soap would be more likely to separate since there will be an increased difference in viscosity/density between soap (bottom layer) and oil portion (top layer), compared to less diluted one where soap and oil portion might have close densities and therefore oil portion stays suspended in the soap..."

I want to say that it's important to not confuse viscosity (syrupy-ness or watery-ness) with density. They can interact with each other, but they are quite different properties.

You can have two materials with the SAME density (weight / volume) and any viscosity. The two won't separate if mixed together. You can have two materials with DIFFERENT densities and any viscosity, and the two will eventually separate if mixed together.

What is affected by viscosity is the rate (speed) of separation. If the primary liquid is viscous and the density difference between the liquids is small, the rate of separation will be very slow. An example would be a soap paste (very viscous!!!) containing too much superfat. If the primary liquid has a thin viscosity and the density difference is large, the separation will be fast (diluted LS with too much superfat).


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