# Liquid soap with cloudy layer on top, clear on bottom



## annie7216 (Jul 30, 2014)

Hi everyone

I know that the range of expertise on this forum can help me understand what I did wrong. I finally tried liquid soap after making cp soap for years. This was my test case recipe:

3.6 oz palm
4.2 oz coconut oil
18 oz soybean oil
6 oz castor oil

6.3 oz KOH
18.9 oz distilled water.

I cooked forever (about 8 hrs) and it was translucent. I diluted (forever again, about 2 days worth) with about 70 oz distilled water. It was thick, but all clumps were gone. 

I used citric acid onlly for neutralization. A 20% solution of which I added 2.5 tablespoons. It curdled upon neutralization then cleared after another day. It was a rich amber color. I then reheated and added lemongrass, orange, and peppermint essential oil to divided doses of the soap. It immediately clouded up. I placed in to sequester and now the peppermint is ok but the other 2 are 3/4 cloudy (top layer) and 1/4 clearish (bottom layer). 

I tried googling this, but I cannot find what it means. I'd really appreciate your expertise. So far, I am not liking liquid soapmaking!

Thanks so much
Annie


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## Susie (Jul 30, 2014)

*Hi Annie!*

As far as I can tell from SoapCalc and SBM lye calculators, you used in the neighborhood of 10% superfat.  It did not need neutralization.  I would pH test it with a reliable meter first, but you might be able to save it with judicious use of a KOH/H2O mixture.  Will give you the link to the thread someone posted a while back in moment.

**EDIT** OK, my search-fu is completely broken.  Can someone help?  Perhaps a DeeAnna rescue?


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## annie7216 (Jul 30, 2014)

*lye calculations*

Hi Susie
Thank you for your reply. I always do my lye calculations by hand, I'm not sure where I went wrong. If anyone would be willing to check my math, I'd be really appreciative.

Palm oil SAP rate = .139 X 3.6 (oz oil) = .50
coconut oil sap rate .252 X 4.2 (oz oil) = 1.0
soybean oil sap rate .188 X 18 (oz oil) = 3.3
castor oil sap rate .179 X 6 (oz oil) = 1.07

add together .5 + 1.0 + 3.3 + 1.07 = 5.87 lye at 0 discount

I wanted to give an 8% excess not a 10% so I multiplied 5.87 X  .08 = .46

I added .46 to 5.87 and got a total of 6.3 lye which I thought was at an 8% lye excess.

I would really really appreciate a check of my math because this is how I make all my soap. Thank you so much.
Anne


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## DeeAnna (Jul 30, 2014)

Palm oil saponification value is .145 for NaOH and .203 for KOH according to my notes.


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## annie7216 (Jul 30, 2014)

*palm oil sap*

Ugh, yes you're right DeeAnna. I had the wrong palm oil sap value. Thank you for checking.
But I'm still not sure it would have been enough of an error to mess up the soap. The lye amount would only have gone up by .2.


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## KristaY (Jul 30, 2014)

Hi Annie! Take a quick look at this thread and see if it's what you're experiencing. My separation was due to fragrance.

http://www.soapmakingforum.com/showthread.php?t=47548


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## seven (Jul 30, 2014)

These are the SAP values I got from soapcalc for KOH:

palm 0.199
coconut 0.257
soy 0.191
castor bean 0.18


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## DeeAnna (Jul 31, 2014)

"...I always do my lye calculations by hand, I'm not sure where I went wrong...."
"...citric acid onlly for neutralization. A 20% solution of which I added 2.5 tablespoons..."
"...The lye amount would only have gone up by .2...."
"...from SoapCalc and SBM lye calculators, you used in the neighborhood of 10% superfat...."

So, okay, from what I'm seeing, the issue is that small errors all add up. Here is a quick check. (Please bear in mind I haven't yet finished my first cuppa joe this morning, so my math might be a bit shaky.)

You added 2.5 TBL of a 20% citric acid solution which is about 0.25 oz citric by weight. That would consume 0.25*6/10*1.403 = 0.2 oz KOH. 

You miscalculated by using the wrong Sap value, so used another 0.2 oz less KOH than required.

By using only 6.3 oz KOH rather than 6.3+0.2+0.2 = 6.7 oz KOH, the error is (6.7-6.3)/6.3*100%=6.3% less KOH than required.

And another issue is that I'm guessing you did not realize when you calculated your recipe is that the KOH we use to make LS is not 100% pure. It is only about 90% to 92% KOH. So that 6.3 oz of purchased KOH is actually only 5.7 oz of 100% KOH. Most of the online soap recipe calculators are set up to take this into account.


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## annie7216 (Aug 1, 2014)

Hi Dee Anna, even without coffee your math is great! Thank you so much for taking the time to help. 
I did know about the KOH being less than 100% pure and did add in (what I thought was) a lye excess of 8% but not 10%. I find it very confusing. Every online calculator gives me a different value that's why I prefer calculations by hand. It seems that some KOH calculators are calibrated to 0 and some are calibrated to a lye excess. I have none of these problems with good old cp soap! Not sure this type of soaping is for me.


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## annie7216 (Aug 1, 2014)

HI seven
I realize that the sap values that I used (from chart on site, from nature with love) appeared to not be rounded up. So I got .188 for soybean which I guess would round up to .19. But I used .18. This also happened for castor oil. I didn't know we were supposed to round them. Thanks for letting me know.


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## annie7216 (Aug 1, 2014)

Kristy
Yes that is exactly what happened to my soap. It was fine before I added the essential oils. I don't understand. Would polysorbate 80 work? Can I use the soap the way it is?


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## PrairieLights (Aug 1, 2014)

Following. 
I had some perfect LS- and the portion scented with EO's separated. I shook it up and 2 weeks later it is still fine. Gosh... I think I am starting to have a theme (had a CP batch separate on me today)


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## DeeAnna (Aug 1, 2014)

"...Every online calculator gives me a different value that's why I prefer calculations by hand...."

Well, yes, that is true. But why are hand calcs any "better"? I'm playing devil's advocate here, by the way, not trying to change what is working for you. 

Think about it -- you had to pick certain saponification values for your hand calculations, right? So your calcs are going to be different than the online recipe calcs. And, yes, each online calc differs, at least a bit, from the others. I'm not sure that is a huge issue, because it's all an educated guess anyway. We really have no idea if the sap values we are using are really the precise sap values for the fats sitting on our kitchen counters ready to be made into soap. The only way to ensure that kind of accuracy is to actually test the saponification value of the actual fats.

Given that the sap values are estimates, hopefully close estimates, but still estimates, my advice is to pick a calc, whether online or one of your own making, and just use it consistently and correctly.

I have created my own spreadsheet soap recipe calculator. I'm not into doing the calculations by hand. I did enough to prove I understood the method and then translated the process into Excel. As you have found out, it's too easy to make mistakes doing it by hand ... and all that repetition is really boring to me!  

My calc takes into account KOH at 92.5% purity based on my supplier's info. It also takes into account NaOH purity at 97%, again based on supplier info, which is something I do not think many soapers worry about. I used as many of soapcalc's sap values as possible for reasonable consistency with soapcalc. That way I can use soapcalc as a double check for accuracy.

"...I didn't know we were supposed to round them...."

For the record, do NOT ever round sap values when doing calculations. Use all three digits all of the time. The only rounding should be on your final lye amount to get the correct number of significant digits for the type of scale you are using. Many people choose to round the final lye number DOWN and round the fat weight UP, all to ensure safety. This isn't the kind of rounding I would teach in my math and computer classes, but it makes perfect sense in the context of soaping.


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## annie7216 (Aug 6, 2014)

Hi DeeAnna
Thank you for your well thought out reply. I guess I thought that sap values, on charts, were all identical, and that online calculators all differed. I was wrong. It would make my life waay simpler if I used an online calculator rather than my hand calculations. I am always worried that I made an error, so I double check and triple check.
Thank for the advice about rounding. I never did before except for the final lye amount, as you suggested. And I too round down.
I really like your idea about an Excel worksheet. That is fabulous. I would still feel like I had the control of my own calculations, but I would lose the error factor! I did take the KOH purity level into account but never worried about the NaOH level, but this is something to consider.
Thanks again.


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## annie7216 (Aug 6, 2014)

Prairie Lights, I too shook up the liquid soap. Now its starting to separate gain, but I think it is slowly going away. Maybe I just need patience. I find that liquid soap is definitely a lesson in patience.


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## KristaY (Aug 6, 2014)

annie7216 said:


> Prairie Lights, I too shook up the liquid soap. Now its starting to separate gain, but I think it is slowly going away. Maybe I just need patience. I find that liquid soap is definitely a lesson in patience.


 
 In my personal experience, once the separation has occurred it will keep separating. I can shake and it'll look great but will eventually fall out of solution again. Has this been the same for others? I'm working to fix it with PS 80 (thanks for that advice, IrishLass!).


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## DeeAnna (Aug 7, 2014)

"...sap values, on charts, were all identical, and that online calculators all differed..."

<chuckle!> Yep, I can appreciate why you thought that. Here are two examples of the fatty acids (FA) in lard. Both sets of numbers are averages of many different individual samples.

FA name	SoapCalc
Capric	na
Lauric	na
Myristic	1
Myristoleic	na
Palmitic	28
Palmitoleic	na
Sapienic	na
Margaric	na
Stearic	13
Oleic	46
Elaidic	na
Ricinoleic	na
Vaccenic	na
Linoleic	6

FA name	ResearchDiets
Capric	0.1
Lauric	0.1
Myristic	1.1
Myristoleic	na
Palmitic	19.4
Palmitoleic	1.4
Sapienic	na
Margaric	0.3
Stearic	10.6
Oleic	33.4
Elaidic	na
Ricinoleic	na
Vaccenic	na
Linoleic	22.4

Just looking at the primary fatty acid -- oleic -- you see that SoapCalc shows 46% oleic and the data from Research Diets shows 33.4% oleic. 

Palmitic varies from 28% in SC to 19.4% in RD. The saponification value of each will be slightly different due to the different fatty acids. 

Quite a difference, hey? They're both legitimate data sources, but the information is radically different. The composition of fat varies with the season, the environmental conditions, the diet (if from an animal), location (palm kernel vs. palm), genetics, etc. 

Which saponification value should you use in hand calculations? Without knowledge of the sap value of YOUR particular lard, I'd probably default to soapcalc's values for no other reason than you can use SoapCalc as a check.

Hope this helps!


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## DeeAnna (Aug 7, 2014)

Here's more. These are the NaOH saponification values for some common soaping fats. I gleaned the data from four different sources -- the Certified Lye company, SoapCalc, The Soap Dish, and Majestic Mountain Sage. SMF is terrible at showing tables in a message, so I've put the info in as an image. You can see the sap values are pretty close for many of the fats, but the sap values for several of the fats vary somewhat -- check out coconut oil!

PS: At the time I did this work, I hadn't yet collected many of the sap values from SoapCalc, but I think the numbers in the table still make my point.


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## KristaY (Aug 7, 2014)

_Quite a difference, hey? They're both legitimate data sources, but the information is radically different. The composition of fat varies with the season, the environmental conditions, the diet (if from an animal), location (palm kernel vs. palm), genetics, etc. _

 Wow. DeeAnna, thank you so much for doing all this research. I've always wondered why I get different amounts of NaOH from different sites when I enter the exact same info into each. Now I know. So basically the sap & NaOH given are a ballpark instead of an exact as I've always thought. If we enter 5% SF for our recipe we may end up higher or lower depending on all the variables. It makes me re-think several of my batches that turned out odd. Maybe one traced differently than one I made a month ago, was brittle or too soft to cut at 24 hours, etc. It may explain why the soaping gremlins visit periodically too. This data tells us it's basically a soaping crap shoot (to a certain extent) when it comes to determining the amount of lye needed. This is one of those "a-ah" moments for me. 

 DeeAnna, you always make me think outside the box which I love. Thanks for that! :-D


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## DeeAnna (Aug 7, 2014)

"...I've always wondered why I get different amounts of NaOH from different sites when I enter the exact same info into each. Now I know. So basically the sap & NaOH given are a ballpark instead of an exact as I've always thought...."

Exactly, Krista! You nailed it. 

Soap recipe calculators are a "model" of reality, as scientists and engineers use the word. Models can be very close representations of the real world, but they are not perfect. In the case of soap recipe calculators, there is some unknown amount of error based on the model-maker's choice of sap values compared with the actual sap values for your real-life fats. 

The point is to take the calculators answers seriously, but just understand there is some error involved. I recommend picking a "model" (a soap recipe calculator) that you like to use best and stick with it. You will learn what superfat and other settings work best for that particular model of reality, so you get the most consistent results as possible.

"...It makes me re-think several of my batches that turned out odd. Maybe one traced differently than one I made a month ago, was brittle or too soft to cut at 24 hours, etc. It may explain why the soaping gremlins visit periodically too..."

Another thing to keep in mind is that it's not only the error in the model that can affect your soaping results. The fats you are using vary in their chemical makeup, and free fatty acids (FFAs) are a particular concern. Soapers really can't see, smell, or otherwise measure FFAs, but FFAs can cause radically unexpected behavior when making soap. 

A fresh oil that has been carefully processed will have a low percentage of FFAs. If you look at the standards, for example, for extra virgin olive oil, olive oil, pomace, and the other grades of olive oil, you'll see one of the requirements for EVOO is a low acid %. Olive oil and pomace are allowed higher acid %'s than EVOO. The "acid" is the FFAs. 

An oil with low FFAs will probably trace relatively slowly and act in a fairly predictable way when making soap. An oil that is older or has been heated too much or is a lower grade oil (pomace) will have a higher percentage of FFAs. This oil may smell and look perfectly fine, but the extra FFAs may cause the batter to trace quicker. At worst, the batter could rice or even seize if the FFAs are high enough.


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## Kyra (Aug 8, 2014)

*Similar recipe also separated*

A very interesting thread, ladies! Thank you all for your input.

Annie, I recently made a very similar recipe (I do not have it in front of me, to check the amounts, but it sounds very close to the one I just made) but I experienced separation after adding the citric acid. I just recently started using citric acid, borax never gives me any kind of issues, but I want to get this citric acid neutralization down. After sitting for almost a week now, the soap has a very cloudy (compact cloudy) layer on top and the bottom is crystal clear. I have some set aside in a plastic bottle (I use it as dish soap) and I mix it back up by shaking it, but after a few hours it separates again. I checked the PH and it is at 8.67.

I guess my question is: is separated soap safe to use? The Ph is good, it foams and cleans beautifully, it is not harsh on my skin, it seems fine, it's just separated.


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## FGOriold (Aug 8, 2014)

Kyra - you took the pH too low with the citric acid (soap is an alklaline product and trying to force the pH down too far, you will cause it to "break" apart).   When you create the soap it takes the oils and lye and turns it into soap + glyceirn + water.  When you lower the pH too far, it reverts back but into fatty acids + potassium citrate + water = no longer "soap".  You probably still have some saponified oils in there as it will not completely break down and will therefore still function - but it may continue to break down over time as you are starting to reverse the saponificaion.  You can raise the pH back up to fix this by adding additional KOH dissolved in a bit of water.  DeeAnna has a formula for doing so - maybe she will chime in.


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## Susie (Aug 8, 2014)

FGOriold said:


> You can raise the pH back up to fix this by adding additional KOH dissolved in a bit of water.  DeeAnna has a formula for doing so - maybe she will chime in.



Yes, please, DeeAnna.  I failed to save that to my soaping files on my computer or print it out when you posted it before.   And, though I have searched, I have been unable to search it out again.   TIA!


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## DeeAnna (Aug 8, 2014)

Is this what y'all are talking about? 

6 g NaOH will be neutralized by 10 g citric acid
8 g KOH will be neutralized by 10 g citric acid

How much citric acid did you use to (over) neutralize your soap? That will give you an upper limit on how much KOH you need to fix the problem. I'd mix that amount of KOH in water, add about half of that solution to your LS, stir, and see what happens. 

The fatty acids you have created should react fairly quickly with KOH (or NaOH) as long as there's enough mixing going on so the KOH and the fatty acids can "find" each other. Obviously you don't want to mix so furiously that you whip up a lot of suds, but you do need to mix well.

Hope this helps!


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## Susie (Aug 8, 2014)

It is actually the "mix X amount of KOH with X amount of water, and add X amount to the soap at the time until it comes back together"  I am looking for, but I copied and pasted the above to refer to later, so thanks!


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## DeeAnna (Aug 8, 2014)

Oh ... I'm afraid that wasn't my advice. Irish Lass perhaps? Not sure.


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## Susie (Aug 8, 2014)

My bad.


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## Kyra (Aug 8, 2014)

Faith, thank you so much for the input. I'll try to do that rather than dumping the gallon of soap I just made. Soybean oil is very expensive here and I would hate to waste such a good soap. It cleans really well, I just need to whip it back into formula. Thanks once again!




FGOriold said:


> Kyra - you took the pH too low with the citric acid (soap is an alklaline product and trying to force the pH down too far, you will cause it to "break" apart).   When you create the soap it takes the oils and lye and turns it into soap + glyceirn + water.  When you lower the pH too far, it reverts back but into fatty acids + potassium citrate + water = no longer "soap".  You probably still have some saponified oils in there as it will not completely break down and will therefore still function - but it may continue to break down over time as you are starting to reverse the saponificaion.  You can raise the pH back up to fix this by adding additional KOH dissolved in a bit of water.  DeeAnna has a formula for doing so - maybe she will chime in.


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## Kyra (Aug 9, 2014)

DeeAnna, thank you so much for your "fix it" formula. I added the KOH solution to my LS and it magically went back into formula. My soap is not crystal clear, it is slightly cloudy, but you can read a paper underneath the testing glass. I am sooo happy I didn't give up on this batch and even more happy I could salvage it. PH is back up to 9.34. Should I higher it some more?

UPDATE: I did add some more KOH solution and got the PH up to 9.49.  




DeeAnna said:


> Is this what y'all are talking about?
> 
> 6 g NaOH will be neutralized by 10 g citric acid
> 8 g KOH will be neutralized by 10 g citric acid
> ...


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## FGOriold (Aug 9, 2014)

Kyra - I would leave it for now and let it sequester for a bit, then reevaluate it.


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## Kyra (Aug 9, 2014)

Faith,

I will do that. More than 5 hours later, it's still not clear, it is still a bit cloudy, but at least it is not separated any longer, no layer is forming on top, which gives me hope. I'll see what a few days of sequestering will do to it. I will recheck the PH after a few days.


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## FGOriold (Aug 9, 2014)

Kyra - there could be other reasons that your soap is a bit cloudy too - oils used, superfat amount, etc.


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## DeeAnna (Aug 9, 2014)

I think Faith has the right of it, to throw my inexperienced opinion into the ring. With soap, liquid or otherwise, there is a lot of stuff going on that just takes time. I can answer many of the general chemistry type of questions, but Faith and Susie are much more experienced at making LS than I am, and I respect their advice and knowledge.


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## Kyra (Aug 9, 2014)

Thanks ladies! I was just reading some tutorials on Faith's site  Yep, I agree, Faith and Susie's expertise in LS  making is a mine gold for the rest of us! So grateful you ladies (all of you!) are sharing the wealth of your knowledge with us!


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## annie7216 (Aug 11, 2014)

*fixing this batch*

Thank you everyone, for all of the very helpful information. My soap is still separated with a cloudy layer on top. I thought it would eventually disperse, but it shows no signs of doing so. I'm going to try to fix this batch by adding in more KOH as suggested by many of you on this forum. 

I'm a little confused though about how much to add. I originally mixed .5 oz of citric acid into 2 oz of water, then added 2 and a half tablespoons of that solution to my soap. However, I didn't use up the entire mixture. I threw some away because it made more than 2 and a half tablespoons. Do I still use .5 oz of KOH? Maybe I'll start with half that amount?

My other problem is that I separated the batch into 4 mason jars. Once I make the KOH solution I'm assuming it would be ok to equally distribute half of it among the  jars? 

Thanks again, for all the help. It takes a village!


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## DeeAnna (Aug 11, 2014)

"...Do I still use .5 oz of KOH? Maybe I'll start with half that amount?..."

Noooooo...... You don't want to use an equal weight of KOH as citric. The relationship is this -- 10 parts citric are neutralized by 8 parts KOH (to get away from weight units).

You put 0.5 oz citric in 2 oz water. What weight of KOH is needed to neutralize 0.5 oz citric? 

0.5 * 8 / 10 = 0.4 oz KOH

Now reverse what you did earlier, except use KOH, not citric: 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. If still more is needed, add 1/2 TBL (1 1/2 tsp). You have now added enough KOH to the LS to neutralize all of the citric you added earlier.

"...Once I make the KOH solution I'm assuming it would be ok to equally distribute half of it among the jars? ..."

I suppose you could, but I personally wouldn't. Way more work and more likelihood of spills and errors. I'd put all of the LS into one container and deal with it all at once. Do you not have an appropriate container that holds a gallon or so?


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## annie7216 (Aug 14, 2014)

Thank you Deanna, for explaining the process to me. I did not quite understand it earlier, as you surmised. 

It's not that I don't have an appropriate contain, I do. It's just that I separated it into 4 mason jars and added different essential oils to each. So I was hoping to save the individual scents, if possible, but I realize that might not be the case.
Thanks again. It's way more complicated than I originally thought. I apreciate all the help.


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## DeeAnna (Aug 14, 2014)

Oh, I see what you mean. In that case, I'd mess with just one quart of LS first -- add 1 tsp to it, stir, see what happens, add another, etc. Then when you know about how much KOH solution you need per quart, you can try dosing the other 3 quarts the same as you did the first quart.


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## annie7216 (Aug 21, 2014)

*It worked!*

Thank you DeeAnna, it worked! My LS is now a rich amber color, and clear. I swore I wouldn't make LS again, but now I'm already thinking about starting a new batch. Funny what a little success will do.

My final question, I hope, is whether the LS is ready to be used or not. Having just added a diluted KOH solution to it, does it need a time period to fully saponify? I did test the LS with ph paper (which I realize is not the best tool since I only get a color indicator for the ph), but it gave me an estimate of 8-9. But because this KOH solution was not subjected to a cooking process, I'm hesitant to use it right away.

Thank you so so much for all the help. It is greatly appreciated.


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## Susie (Aug 21, 2014)

It is good to go now.  That is the beauty of LS.  No 4-6 week waiting to try it.

Congratulations!


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## DeeAnna (Aug 22, 2014)

Good for you! Glad to hear adding a bit of KOH solved the problem.


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