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Safety of BDG soap, FDA information, Therapeutic Claims and Labeling
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That sounds about right, Mine is about the same and I started loosing purity only after I added the vacuum, or when I was able to get the temp in the 350*F range without smoking.


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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quote:
Originally posted by Rick K:
That sounds about right, Mine is about the same and I started loosing purity only after I added the vacuum, or when I was able to get the temp in the 350*F range without smoking.


I haven't quite got my head wrapped around how to introduce vacuum into my setup and still maintain high purity, seems like some water vapor would get sucked through. Plus would probably collapse the drum rather easily.

Since I keep the water in the glycerin I would think it would lower the methanol ppm even more. I'm satisfied that its low enough in the final form as the soap but perhaps I'll try to find someone local with a GC just to satisfy my curiosity.

What are your ppm numbers in the finished product?



 
Registered: April 28, 2008Reply With QuoteReport This Post
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I'm researching the vacuum questions right now, I am more concerned with removing the methanol from the BDG than the methanol purity.

I think all I am going to have to do is beef up the reflux column, under vacuum it comes out much faster at lower pot temperatures.

If you dilute your soap at all that will also lower the PPM of methanol.

Methanol content in my soap was .08%.


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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rick, your methanol content is higher than I thought it would be. personally, i'd consider .08% significant. I haven't had mine tested, but I need to.

I have a few thoughts. the methanol should continue to evaporate as the soap cures. especially where i'm located in the tropics. the water is certainly evaporating during the cure process, that tells me that the methanol is evaporating even more so. I'm not too concerned about the exact amount of methanol in the glycerin by-product, but more concerned about how much is left in the bars.

I'd like to test one of my newly produced bars and one that's cured for 6 weeks. I would bet my results would be significantly different between the two. A 6 week cure gets my bars rock hard, so hopefully that means negligible methanol content. If that is the case, than I'm not going to worry too much about how much methanol is left in my glycerin and I'll maintain my current distilling procedure.

You may have mentioned it, but where are you getting your methanol content tested?
 
Location: earth | Registered: November 23, 2005Reply With QuoteReport This Post
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Yes, And that's why I really think all of us making BDG soaps need to have them tested for methanol content.

Another BDG soaper had hers recently tested at .6% that's why I started questioning our assumptions and re-researching what is acceptable.

But .08% is very much lower than the 4% that the glycerin starts with after methanol distillation, provided that that chart is correct. And according to the chart to get the methanol down as far as I have you would have to heat the BDG to between 400*F and 500*F. This test was from soap that I had just finished I need to send one out that has aged.

I am not sure that curing will evaporate methanol like you think it will. Just like if we set the glycerin out in a bucket that will not remove the methanol. However with transparent soaps using ethanol they claim it does evaporate and becomes an incidental ingredient.

Rock hard is an indication of the primo palm kernel/coconut BDG you have. During the cure time any excess water and possibly methanol will evaporate.

The liquid soap most likely will not evaporate during curing, however if they are diluted that will significantly lower the PPM of methanol.

I will know more after I send in the series of BDG tests for methanol testing.

I think that the methanol content in the BDG is most important part of the process. The lower it is after methanol distillation the lower it will be after making the soap. According to that chart it takes over 500*F before it gets down to 0.


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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That is the case until you start getting an azeotrope of water and methanol as the head temperature rises above 159*F.

There is no azeotrope with methanol and water, 100% purity is very achievable unlike the situation with ethanol.
In my experience with vacuum it does not behave like you may think, once the initial air is sucked out of the tank at around 5~10Hg the amount of vapor being sucked through the condenser slows down dramatically as there is not much there to be sucked past it. If you can attach a hose to the output of your vac pump and put it in a pail of water you can easily witness this by the amount of air coming out the hose. With vacuum the size of the column could likely be quite a bit smaller than when using a traditional pot still. IMO of course. I found that the most important part is to regulate the vacuum so as not to overload the condenser, I just use a small needle valve to let air in at the pump so I can slowly ramp up the vacuum without overloading my condenser.
You can see my regulator in this picture between the pump and the gauge:

That little 2 dollar valve is the most important part of my recovery to prevent overloading the condenser.
Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post



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Oh man how cool is that!

Thanks' Jon, I think you just saved me a bunch of headaches!


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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quote:
Originally posted by freesoul:
quote:
Originally posted by Rick K:
The starting percentage of the methanol has nothing to do with how much is left after distillation. Distillation has to do with vapor pressure and temperature. The "pot" temperature will not rise until enough distillate is removed for the vapor pressure to change. If you heat the BDG to 288*F and the chart that is commonly referenced is accurate there will be 5% methanol left in the BDG.



My question was how can that chart possibly be accurate if it claims a starting value of 45% methanol content at 172F when everything I have ever read was that there was approximately 20% methanol in the glycerin?

Freesoul

My feeling about your question is twofold:
Firstly the chart appears to have been generated by simulation software such as Hysis or Chemcad or similar. It is the kind of software that chemical and process engineers use to simulate a process and come up with a plant design. The reason, I think, the list starts at 45% is simply that this is all that the original poster displayed. What I believe the chart is based upon is a mixture of pure Glycerine and pure Methanol starting at 0% and going all the way to 100% so if the person who ran the simulation showed the complete chart you would have seen it start at 100% methanol/ 0% glycerol going all the way to 0% methanol/100% glycerol. It just happened that he picked 45% methanol as the starting point for display.
Secondly you need to be a little careful with simulation outputs and make sure that you are looking at exactly what has been simulated. Now I don't know what was actually used for the simulation but my guess is that the "Glycerol" that each Biodiesel producer will used wil vary slightly to what was in the simulation. If the person running the simulation assumed that the glycerine was pure but did not account for the fats, esters, mono glycerides, di glycerides, water and salts etc. then the simulated temperatures would need to be proven rather than taken as gospel.

Therefore, in my opinion, no one should rely on the chart as posted to say >290F guarantees less than 5% methanol as that is a dangerous assumption to make as everyone's biodiesel glycerine is likely to be a differnt composition depending upon how the process it.
 
Location: East Yorkshire | Registered: January 14, 2006Reply With QuoteReport This Post
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Originally posted by Rick K:
According to that chart it takes over 500*F before it gets down to 0.

Further to my previous post, yes, the simulated chart shows 500F before all methanol is out. However I assume that is based upon atmospheric pressure distillation, and again based upon pure glycerine with no contaminants.
Don't rely on the chart unless you know the full details of the simulation/ assumptions used.
 
Location: East Yorkshire | Registered: January 14, 2006Reply With QuoteReport This Post
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Good points Fuzznag...
I am sending my glycerin in for actual methanol testing at different temperatures. This will be a good ball park number but from what you are saying it could be different for each batch because of the other "stuff" in the BDG.

So this leads us back to the OP. I think we need to find out at what point methanol becomes safe in soap and further at what point does it become an incidental ingredient.

Then I IMO the final soaps we are making need to be tested to be sure we are within those limits.

It's good to know how that chart was derived.


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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Originally posted by Rick K:
Since methanol will start evaporating out of a 45% solution at 172*F and our methanol concentration is 20% - 30% you should not get any distillate until the temperature gets above 197*F for 25% or 207*F for 20% methanol. This kind of holds true when I am distilling the methanol. But now that I use vacuum distillation the temperatures are different. I typically recover 25% - 30% methanol back during distillation. However the purity goes down as the temperature goes up -- this is because if there is any water in the BDG it is also evaporating.

Rick K
I think you are getting confused between "boiling point" and the point at which something starts to evaporate.
It is incorrect to say that "methanol will start to evaporate from a 45% solution in glycerol at 172F". The chart tells you the boiling point, not the point at which methanol start to evaporate.

There is a big difference between boiling point and the point at which something starts to evaporate. Just to clarify using water as an example, the boiling point of water is 100C(212F) but when it rains the water on the sidewalk evaporates even though the ambient temperature never reaches 100C(212F)

This is the same for the methanol in the chart, methanol will be evaporating from a very low temperature however the chart is simply showing you that the whole mixture will be boiling at the temperatures shown. So if you heat up your BDG to 172F then if there is a 45% methanol content it will be boiling, however if there is less methanol then it is likely not to be boiling but it does not mean that methanol has stopped evaporating.
 
Location: East Yorkshire | Registered: January 14, 2006Reply With QuoteReport This Post
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quote:
Originally posted by Rick K:
Good points Fuzznag...
I am sending my glycerin in for actual methanol testing at different temperatures. This will be a good ball park number but from what you are saying it could be different for each batch because of the other "stuff" in the BDG.

So this leads us back to the OP. I think we need to find out at what point methanol becomes safe in soap and further at what point does it become an incidental ingredient.

Then I IMO the final soaps we are making need to be tested to be sure we are within those limits.

It's good to know how that chart was derived.
Yes, I agree, it all depends upon the mixture of components that you start with and how they affect the methanol evaporation.

But yes, it would be good for someone to find out what the limits of methanol in soap should be especially as the finished product is being sold to Joe Public.
 
Location: East Yorkshire | Registered: January 14, 2006Reply With QuoteReport This Post



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quote:
Originally posted by Fuzznag:

Rick K
I think you are getting confused between "boiling point" and the point at which something starts to evaporate.
It is incorrect to say that "methanol will start to evaporate from a 45% solution in glycerol at 172F". The chart tells you the boiling point, not the point at which methanol start to evaporate.


I was just trying to say that if Freesouls BDG has 20% methanol he may not see much methanol coming out at 172*F. But that is not an indication of the chart being inaccurate or accurate for that matter.

But yes you can have evaporation without something boiling.


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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quote:
Originally posted by Fuzznag:
Yes, I agree, it all depends upon the mixture of components that you start with and how they affect the methanol evaporation.

But yes, it would be good for someone to find out what the limits of methanol in soap should be especially as the finished product is being sold to Joe Public.


That's why I started this post, hopefully one of us can come up with a definitive answer.

Minimally what we know is that over 4% is considered dangerous and needs special labeling according to the Consumer Product Safety Commission.

BWilder found that in Canada it is 1%.

Once I get some of the BDG tests back we will have a better idea of how accurate that chart is in general, knowing each time testing is done it could vary some.


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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The FDA maximum for methanol in wine is 0.1%
 
Registered: November 22, 2010Reply With QuoteReport This Post
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Oh that is GREAT to know!
So I would think that if we were under that topically we should be safe.

Not to say we shouldn't keep trying to get it as low as possible...


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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Been following this thread intently. So if we take that .1% as the max allowable for topical use(an assumption) that would translate to 1000ppm. Chances are, if there is such a regulation(or to be created) for topical use, it probably is(would be) somewhat higher(say maybe 4-5x). Would think that it would be related to absorbtion rate through skin, and expected contact time. Recall the 5% limit for the toxic labeling - one could argue that anything below that is not considered toxic by the gov. and is safe. Whether 5% is considered safe(meaning no detremental effects), I can't say. Still, I'd rather the soap I use to be closer to 1000ppm(.1%) than 5% given what even limited exposure to higher concenttations can result in. What ever the official numbers are(or will be), they're still a guess, but at least it's a considered & thought about number that is probably conservative in the minds(Who should have more knowledge & experience in the pertinent fields than I do.) of those making the recommendation/decision.

I'd use the chart as a rule of thumb, for testing finished glycerol that I'm going to use to make soap, not as a guide as to how hot I have to make my glycerol while demething it.
 
Location: Santa Cruz, Ca | Registered: July 29, 2006Reply With QuoteReport This Post
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Am I the only one that sees the elephant in the room here? How long has biodiesel glycerin soap been claimed to be made, even sold in "kits" and yet ONLY NOW is its safety being discussed ?

I've had methanol level safety information in my Ebook, The Guide, for several YEARS now, long before I ever made any soap that saw its way into public hands. Is this an information thread or getting someone else to do research that obviously hasn't been done?



** Biodiesel Glycerine Soap - The Guide
- on 5 continents helping people make & sell soap from the Biodiesel Glycerine.


 
Location: :-) Great White North eh ? | Registered: December 10, 2004Reply With QuoteReport This Post



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Methanol safety is being re-visited as new information becomes available.

Recent conversations with the Consumer Product Safety Commission have pointed out that according to 16CFR1500.14 over 4% methanol in any product is toxic and needs special labeling and packaging. Heating the BDG to 260*F will contain over 5% methanol -- according to the chart that is commonly referenced on this forum. We use a safer temperature of 300*F - 350*F but this still may be to close to the 4%.

quote:


(4) Methyl alcohol (methanol). Because death and blindness can result from the ingestion of methyl alcohol, the label for this substance and for mixtures containing 4 percent or more by weight of this substance shall include the signal word ‘‘danger,’’ the additional word ‘‘poison,’’ and the skull and crossbones symbol. The statement of hazard shall include ‘‘Vapor harmful’’ and ‘‘May be fatal or cause blindness if swallowed.’’ The label shall also bear the statement ‘‘Cannot be made nonpoisonous.’’



I am sending out BDG samples at various temperatures with and without vacuum to get an actual indication of methanol content in our BDG. Once I get those we will find out how accurate that chart is with real world BDG. The methanol in BDG chart will be published in "Making Biodiesel Soaps" replacing the current methanol safety information contained there. Here's hoping that the current chart is off and the methanol content is lower than expected at the various temperatures.

Methanol safety is just as important as testing for caustic soap. Those are the two most important items a BDG soaper should concern themselves with.

This is not to mean that one should not have their soaps tested for methanol content -- methanol testing is a responsible way to be sure your BDG and end product soaps fall far under just "acceptable".

Just pushing the envelope and making sure that inaccurate information is replaced with accurate information.


-Rick

http://www.knicenclean.com your single-most largest free BDG soaping content on the internet.
SAP Testing, Ingredient Properties, Soap Glossary and Recipes just to name a few.

Making Biodiesel Byproduct Soap Learn how to use your biodiesel byproducts to make great bar and liquid soap!!!

"Closing the loop on biodiesel production one bar at a time!"

Beware of the Dunning–Kruger effect.
 
Location: S.E. Michigan | Registered: April 15, 2007Reply With QuoteReport This Post
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Originally posted by Rick K:
Methanol safety is being re-visited as new information becomes available.

Recent conversations with the Consumer Product Safety Commission have pointed out that according to 16CFR1500.14 over 4% methanol in any product is toxic and needs special labeling and packaging. Heating the BDG to 260*F will contain over 5% methanol -- according to the chart that is commonly referenced on this forum. We use a safer temperature of 300*F - 350*F but this still may be to close to the 4%.

Rick

I think you are still confused regarding the chart that you keep referencing and the percentage of methanol it shows.

The chart is simply indicating the boiling point of the mixture it is not telling you how much methanol is left after reaching that temperature and it should not be viewed in that way as it is creating a false belief in residual methanol content that you keep refering to.

The amount of methanol remaining in your glycerol is all about evaporation and time not boiling you don't need to reach the boiling point for the methanol to evaporate but it would evaporate faster if it was boiling
 
Location: East Yorkshire | Registered: January 14, 2006Reply With QuoteReport This Post
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