CPLS batter separates from water

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Hellow everyone!
I started a batch of liquid soap as below:
water300 g
KOH Weight93.57 g at 98% Purity
Sunflower500 g
Fragrance Oil Weight15 g
Superfat0%
Citric acid 30g

I poured the lye water+ citric acid solution in the oil and started blending the batter. While blending, it seemed too oily, so I checked the scale and I realized it had been tared wrong when weighing oil. I ran the difference through the calculator and added 8 more grams of KOH. It seemed to emulsify well, it reached trace, so I set it to rest.

After a short while, I checked it again and noticed some of the water separated and deposited at the bottom. I suppose it might be unsaponified lye water, but since I tried fixing it already and it didn't work, I'm afraid to experiment with it now. At this point I'm not even sure if the scale was wrong, if the citric acid is responsible or what else I might have done wrong!
Any tips?

Cheers!
Romi
 
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gww

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Romi
I do not know if you are hot processing or cold processing and I have only made two batches in my life by cold process. If it helps, I blended mine to a very thick paste and then set it in an oven and checked on it about an hour later and it had some separation but just mixed it as best I could and put it back in and it ate all the stuff that had separated out. I thought it might be a fluke but the second batch did the same. I wonder that it might not have sucked the stuff back in on its own with time but know that it worked stirring and smashing it all together and it all came out good in the end.
Being new, I hope this helps more then hurts and smarter people may call me out on it soon but thought I would put it out there.
Good luck
gww
 

ResolvableOwl

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@Romiriam
A few remarks:
  • Where have you got 98% pure KOH from? That's pretty hard to find; even reputable fine chemicals companies rarely sell >95% KOH, and then at immense prices
  • Does the recipe, like you've inlcuded it above, include the 8 g extra KOH? If yes, then you're more around 3% SF; if not, then you're at 11% SF.
  • But it gets worse, if you added the citric acid just as-is, without increasing KOH as well. You would need 24.5 g extra KOH for the citric acid, otherwise you end up with some 29% superfat (!). No surprise that it might have looked to oily.
  • Figuring out when emulsion is stable and when not is tricky in CPLS, certainly trickier than in CP bar soap. I've had some separation/settling issues, but got them solved by repeated stirring. You want everything to be incorporated, so that all the lye has a chance to reach all the oils, at every place throughout the whole container. Stirring/SBing (if not already too thick) is okay and probably fixes your separation. However, it does not help you with your missing lye.
  • No idea about the FO. It might not have any impact, or it might make everything much more complicated than it already is. I'm not an expert on FOs in LS, but I'd guess it would be better to wait with FO addition until paste dilution.
 

gww

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I told you somebody smarter would probably come along which I am thankful for as I can learn right along with you.
Cheers
gww
 
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@Romiriam
A few remarks:
  • Where have you got 98% pure KOH from? That's pretty hard to find; even reputable fine chemicals companies rarely sell >95% KOH, and then at immense prices
  • Does the recipe, like you've inlcuded it above, include the 8 g extra KOH? If yes, then you're more around 3% SF; if not, then you're at 11% SF.
  • But it gets worse, if you added the citric acid just as-is, without increasing KOH as well. You would need 24.5 g extra KOH for the citric acid, otherwise you end up with some 29% superfat (!). No surprise that it might have looked to oily.
  • Figuring out when emulsion is stable and when not is tricky in CPLS, certainly trickier than in CP bar soap. I've had some separation/settling issues, but got them solved by repeated stirring. You want everything to be incorporated, so that all the lye has a chance to reach all the oils, at every place throughout the whole container. Stirring/SBing (if not already too thick) is okay and probably fixes your separation. However, it does not help you with your missing lye.
  • No idea about the FO. It might not have any impact, or it might make everything much more complicated than it already is. I'm not an expert on FOs in LS, but I'd guess it would be better to wait with FO addition until paste dilution.
That is some interesting information!
The KOH I have reads 99.5% purity on the label, but I guess that's bs and I'll have to consider it a 90% from now on.

I used soap making friend as a calculator and did not see anywhere where I should have fixed KOH quantities when adding citric acid, good to know!
In total I think I put 101g of KOH (I added some more), but I'm now thinking it really might be lye heavy rather than lacking lye.
I have dissolved citric acid in water and then added it to the lye water solution.

The picture is my batter separating shortly after stirring. The dark streaks are lye water, not oil(I think). Since it's not getting any thicker, I might leave it overnight and see if with a good blend on my stovetop it'll incorporate properly...
Thank you for the advice!
 

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ResolvableOwl

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leave it overnight
That's the best advice for CPLS anyway. CPLS is such a sympathic method! 😜

I'm now thinking it really might be lye heavy rather than lacking lye.
The zap test and the dilution test will tell you … tomorrow.

I used soap making friend as a calculator and did not see anywhere where I should have fixed KOH quantities when adding citric acid, good to know!
SMFriend actually has a category for citric acid, down below in the “Custom Additives” section, but its use is discouraged since the math behind it is somehow off.


I'll crawl through your numbers tomorrow again, and we'll see how to fix it then (if necessary).
 
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Couple of things:

1. Definitely do not add the FO at the time of making paste. It is added at dilution. Even then, it needs an emulsifier such as PS80 so it won't separate out of your diluted LS mixture. The separation you are probably seeing is from the FO.

2. Unless you are pretty experienced with LS, I also wouldn't add the citric acid when making the paste. Keep it pretty simple - oils and KOH - until you know what ingredients will affect your paste, and how.
 
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1. Definitely do not add the FO at the time of making paste. It is added at dilution.

I've added FO at paste making every time I made LS before, I made LS 3 or 4 times now. Nothing like this happened before, so I think it might be the Citric acid.

There's a thick layer of separated liquid down there, I checked if it mixes with water and some of it might be oil but definitely not all of it.


How to fix it? Add KOH? Cook it? Both?
 

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ResolvableOwl

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That's a good source, which explains the whys and hows of citric acid in a correct and easily understandable way!

I'll crawl through your numbers tomorrow again
Based on pure KOH & no SF:
500 g sunflower oil (K-SAP 0.189) need 94.5 g KOH
30 g citric acid (anhydrous) need 26.3 g KOH
30 g citric acid (monohydrate) need 24.0 g KOH (I'll assume you've got the monohydrate)
FO: ??? (some components of fragrance oils can consume lye)

Sum: 118.5 g hypothetical pure KOH

That's 119.1 g of KOH at 99.5% purity
Or 124.8 g of KOH at 95% purity
Or 131.7 g of KOH at 90% purity

If you've added mere 101 g, you're at least short of 18 g KOH.
Steps: First, give your paste-in-spe a thorough mix (incorporate the watery bottom layer as good as possible). Then make a clarity test (take out a bit of the paste and dissolve it in 10…50 times its weight in distilled water); from the math it should become murky, maybe even with oil drops floating around. Pour back the clarity test solution into the main batch.
Take some 50 mL distilled water and dissolve 18 g KOH into it. Once dissolved (doesn't need to be cooled down), whisk it into the main batter (no splashing).
Wait one day, repeat the clarity test. (stir if separation occurs again).
 
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FO: ??? (some components of fragrance oils can consume lye)

I used lavander essential oil!

Steps: First, give your paste-in-spe a thorough mix (incorporate the watery bottom layer as good as possible). Then make a clarity test (take out a bit of the paste and dissolve it in 10…50 times its weight in distilled water); from the math it should become murky, maybe even with oil drops floating around. Pour back the clarity test solution into the main batch.
Take some 50 mL distilled water and dissolve 18 g KOH into it. Once dissolved (doesn't need to be cooled down), whisk it into the main batter (no splashing).
Wait one day, repeat the clarity test. (stir if separation occurs again).

Blended it all, added Koh after proper calculations, then blended it again. It already thickened more. The package of my store bought citric acid doesn't specify whether it is monohydrate or anhydrous.
Left a bit of batter in a glass for 30 min to see if it would separate, and it didn't. Yay!

Cooked the batter to force saponification a bit until it turned slightly translucent. It's a lot more fluid than I'm used to, but probably because I added water twice (when I added Koh yesterday and today).
Did a clarity test, very murky but no oil on top. Blended it back in, I'll let it sit for a day and repeat clarity test. Then I think I'll let it sequester on its own.
It looks like this might work out! It's for personal use anyway, so I'm not worried about clarity.
Thank you so much for your help!
 

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ResolvableOwl

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I used lavander essential oil!
Lavender is in fact one of the fragrances that will eat up lye. The 40/42 standard lavender contains 42% linalyl acetate, and hence the EO has a K-SAP of around 0.12 all by itself (ca. 2 g KOH consumption for your batch), and the scent profile changes in contact with lye. In LS, you have the luxury to add the scent well after saponification has finished, better do it that way next time. 😉

But glad to see how this slowly but steadily turns into a success!
 
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In LS, you have the luxury to add the scent well after saponification has finished, better do it that way next time. 😉
Great advice!
I always add my scents after complete saponification and the soap has been diluted.
That just how I do it however, it's not a liquid soap gospel etched in granite by any means.
 
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Great advice!
I always add my scents after complete saponification and the soap has been diluted.
That just how I do it however, it's not a liquid soap gospel etched in granite by any means.
But since FOs and EOs are known to frequently cause separation in LS, is it worth it to risk the batch by adding the FO up front? Adding it later also means that the EO won't be dissipating from the paste during storage (assuming one is making enough to use some now, and store some for later).
 

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