Soaps/Acetone

[1958steveflying]

Results from this test may have to wait until the next batch s I'm having some problems with the titrated soap tests.

The confusing thing is the 50/50 test done after the acid wash was Crystal clear
The same goes with the first and second washes.
The titrated soap tests are also giving confusing results,
124.64ppm after the acid wash,
54.72ppm after wash 1
94.24 after wash 2.
wash 3 is settling as I type.

I can't believe my bio is this good as making soap is something I'm good at.

Did you use Acetone at all in washes 1, 2 and 3?

Now the other tests were done on bio that had been heated in a frying pan to drive off the water before doing the titrated soap test, this must of had an effect on the soaps, but I can't understand why.

Drying the first wash will drive of Methanol that will not wash out in 1 wash, a soap test on that would have to be shaken to death to make sure any dropping soap is still suspended equally. And the same for subsequent washes until the Meth is actually all washed out.

I see what you mean, but it only makes a difference with the 50/50 tests, titrated soap tests should still work.

But if you take a sample and dry it, then it sits until you take your tiny soap test sample off the top then it wont contain the same level of soap that will be at the bottom.  Does that make sense.

Yes it makes sense, but I dried 50ml, cooled it straight away, poured it into a jar and took 12ml from the top, all this was in less than 1 Minuit so no chance for the soap to drop.

I suppose the only way to be sure is to take the 12ml from the bottom of the sample.

[Head Womble]

Results from this test may have to wait until the next batch s I'm having some problems with the titrated soap tests.

The confusing thing is the 50/50 test done after the acid wash was Crystal clear
The same goes with the first and second washes.
The titrated soap tests are also giving confusing results,
124.64ppm after the acid wash,
54.72ppm after wash 1
94.24 after wash 2.
wash 3 is settling as I type.

I can't believe my bio is this good as making soap is something I'm good at.

I've retested wash No1 and got a result of 72.96, previously it was 54.72.

Wash No3 tested at 59.24
I've yet to test wash No4

Now I have something that's bothering me, hopefully Nige or Paul can help on this one,
when doing an acid wash will this interfear with the titrated soap test results,
as I see it we neutralise the veg oil by transestification,
then we add acid to the first wash to neutralise the soap,
does this interfear with the titrated soap test or does all the acid get removed with the wash water.

For these tests would it be better to skip the acid wash,
I know Vince and others pump wash with the acid and don't form emulsions,
I'm sure this is down to the non titration method not producing excess soap
so maybe I can forgo this step for the sake of the testing.

[nathanrobo]

The acid doesn't neutralise soaps, it's the excess lye which has high ph, that we're neutralising. This means no further soaps form due to adding water. Therefore all the soaps that we are needing to wash out, is those produced by converting free fatty acids.

[Jamesrl]

The acid doesn't neutralise soaps, it's the excess lye which has high ph, that we're neutralising. This means no further soaps form due to adding water. Therefore all the soaps that we are needing to wash out, is those produced by converting free fatty acids.

Now correct me if I'm wrong but apart from the titration quantity of lye that gets consumed by saponification ALL the caustic is discharged with the glyc.

I was under the impression that the acid was used to seriously reduce the soaps thus preventing emulsions forming when water is added. 

[Julian]

The acid doesn't neutralise soaps, it's the excess lye which has high ph, that we're neutralising. This means no further soaps form due to adding water. Therefore all the soaps that we are needing to wash out, is those produced by converting free fatty acids.

Now correct me if I'm wrong but apart from the titration quantity of lye that gets consumed by saponification ALL the caustic is discharged with the glyc.

I was under the impression that the acid was used to seriously reduce the soaps thus preventing emulsions forming when water is added.

Me too.

[Head Womble]

Well I've finished the test batch, however the results aren't as clear as I would have liked.
 
The titrated soap tests haven't given consistant results, at some stages I've done three tests and had differing outcomes in each.

Due to this the results from this batch are not going on the wiki page.

That said, even though the results were a little erratic, it has still shown that 1 x acetone wash is as effective as 4 x standard washes using the pimp washing method.

I will repeat this test on my next batch as I have ordered some fresh IPA from Basic chemicals,
hopefully I'll get more accurate results and they can be added to the wiki page.

[1958steveflying]

Well I've finished the test batch, however the results aren't as clear as I would have liked.
 
The titrated soap tests haven't given consistant results, at some stages I've done three tests and had differing outcomes in each.

Due to this the results from this batch are not going on the wiki page.

That said, even though the results were a little erratic, it has still shown that 1 x acetone wash is as effective as 4 x standard washes using the pimp washing method.

I will repeat this test on my next batch as I have ordered some fresh IPA from Basic chemicals,
hopefully I'll get more accurate results and they can be added to the wiki page.

That is really good news Mark, what we knew was happening in practise is now proven. Well done.

[1958steveflying]

The acid doesn't neutralise soaps, it's the excess lye which has high ph, that we're neutralising. This means no further soaps form due to adding water. Therefore all the soaps that we are needing to wash out, is those produced by converting free fatty acids.

Now correct me if I'm wrong but apart from the titration quantity of lye that gets consumed by saponification ALL the caustic is discharged with the glyc.

I was under the impression that the acid was used to seriously reduce the soaps thus preventing emulsions forming when water is added.

Just an observation side note that until demethed a good few litres of glyc still remain in the Bio.

[Head Womble]

The acid doesn't neutralise soaps, it's the excess lye which has high ph, that we're neutralising. This means no further soaps form due to adding water. Therefore all the soaps that we are needing to wash out, is those produced by converting free fatty acids.

Now correct me if I'm wrong but apart from the titration quantity of lye that gets consumed by saponification ALL the caustic is discharged with the glyc.

I was under the impression that the acid was used to seriously reduce the soaps thus preventing emulsions forming when water is added.

Just an observation side note that until demethed a good few litres of glyc still remain in the Bio.

I'd say that even after demething the bio still contains a suprising amount of gyl, the bottom of my settling drum used to have layers of gly then soap.

I'd say a good amount of the creaminess we see in our wash water is actually gly not soap.

[1958steveflying]

The acid doesn't neutralise soaps, it's the excess lye which has high ph, that we're neutralising. This means no further soaps form due to adding water. Therefore all the soaps that we are needing to wash out, is those produced by converting free fatty acids.

Now correct me if I'm wrong but apart from the titration quantity of lye that gets consumed by saponification ALL the caustic is discharged with the glyc.

I was under the impression that the acid was used to seriously reduce the soaps thus preventing emulsions forming when water is added.

Just an observation side note that until demethed a good few litres of glyc still remain in the Bio.

I'd say that even after demething the bio still contains a suprising amount of gyl, the bottom of my settling drum used to have layers of gly then soap.

I'd say a good amount of the creaminess we see in our wash water is actually gly not soap.

That is a good point Mark, there is a but though. lol.. the batch I made using Acetone dropped about all of its Glyc after demething, I didn't manage to get more than a tea spoonful after and that was in the fuge.

[Carrington]

Just very quick
Can you mix a small amount if bio with acetone maybe 50/50 and see if any Glyc drops out then.
This could be a start of a new test system. Haven't realy thought about it but surely any Glyc would drop into a saperate phase. I'm working on spine thing similar with my proces.

[Head Womble]

The acid doesn't neutralise soaps, it's the excess lye which has high ph, that we're neutralising. This means no further soaps form due to adding water. Therefore all the soaps that we are needing to wash out, is those produced by converting free fatty acids.

Now correct me if I'm wrong but apart from the titration quantity of lye that gets consumed by saponification ALL the caustic is discharged with the glyc.

I was under the impression that the acid was used to seriously reduce the soaps thus preventing emulsions forming when water is added.

Just an observation side note that until demethed a good few litres of glyc still remain in the Bio.

I'd say that even after demething the bio still contains a suprising amount of gyl, the bottom of my settling drum used to have layers of gly then soap.

I'd say a good amount of the creaminess we see in our wash water is actually gly not soap.

That is a good point Mark, there is a but though. lol.. the batch I made using Acetone dropped about all of its Glyc after demething, I didn't manage to get more than a tea spoonful after and that was in the fuge.

But you're now talking about an acetone reaction, and that, I supect, is a differant animal altogether.

[nathanrobo]

The acid doesn't neutralise soaps, it's the excess lye which has high ph, that we're neutralising. This means no further soaps form due to adding water. Therefore all the soaps that we are needing to wash out, is those produced by converting free fatty acids.

Now correct me if I'm wrong but apart from the titration quantity of lye that gets consumed by saponification ALL the caustic is discharged with the glyc.

I was under the impression that the acid was used to seriously reduce the soaps thus preventing emulsions forming when water is added.

B good if a chemist type could chime in and define this.  Bio often pre-neutralisation has a high PH due to the presence of lye?  Soaps are present due to the neutralisation of ffa - all agreed about this! These soaps still exist after neutralisation, this shouldn't be too controversial!

Ergo we're neutralising the lye so as not to make significantly more soaps as a result of adding water??  If my understanding is right, using this method, we still have soaps, but only those resulting from the FFA's in the feedstock.  The level shouldn't be high enough to cause emulsification. 

[Jamesrl]

B good if a chemist type could chime in and define this.  Bio often pre-neutralisation has a high PH due to the presence of lye?  Soaps are present due to the neutralisation of ffa - all agreed about this! These soaps still exist after neutralisation, this shouldn't be too controversial!

Err, I think you may have the wrong idea as to what the lye does. It's a catalyst.

A catalyst is NOT consumed in the reaction but the lye over the base number is used to neutralize the FFA in the WVO which results in soap.

The converted and finished bio should be Ph 7, be it water washed to remove the soaps or demethed and settled.

Adding Acid to to the wash water neutralizes the soaps mono and di-glycerides.

[Carrington]

B good if a chemist type could chime in and define this.  Bio often pre-neutralisation has a high PH due to the presence of lye?  Soaps are present due to the neutralisation of ffa - all agreed about this! These soaps still exist after neutralisation, this shouldn't be too controversial!

Err, I think you may have the wrong idea as to what the lye does. It's a catalyst.

A catalyst is NOT consumed in the reaction but the lye over the base number is used to neutralize the FFA in the WVO which results in soap.

The converted and finished bio should be Ph 7, be it water washed to remove the soaps or demethed and settled.

Adding Acid to to the wash water neutralizes the soaps mono and di-glycerides.

As you say Jim the catylist is not consumed so therefor is still available to make soap if water is added , by adding acid this then kills the catylist preventing it from being able to create soap when water is added.
The bio should be ph7 as the catylist doesn't disolve in the oil or bio but it still floats about in the mix until washed or settled out
So the bio is ph7 but the mix could be up as high as 12-14