Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: 1958steveflying on December 23, 2012, 05:57:45 PM
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Okay I am going to throw this out there after just one brain/wave/fart ! !
Today I had a sample of my latest acid neutralised water washed Bio (sparkling example), I did a 50/50 test on it and it split quickly with no line in between and pretty much clear water.
Now Nathan and I were chewing the cud over all sorts and Acetone came into the fore. So I thought I wonder if Acetone added to the wash water may help soaps splitting out as it has an effect on surface tension etc etc.
A drip was added to this sample and shaken again... resulting in very murky water this time around. (A drip of Acetone was added to just water to see if it went murky and it did not).
Now I have one of Nige's soap testing kits but have never tried or got my head around it as I am useless at colour changes and figure this is a necessity.
Anyone care to take on a bit of further experimenting ?
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You bet Steve bring it on
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This is what I homebrewing is about! Ideas and experiments.
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I have one of Nige's test kits and also some acetone.
I'll do some small tests after Christmass and post the results.
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Nice one. I wonder if it would also help settling with standard demeth and settle process or whether water is key here (I'm guessing a polar solvent like water is needed).
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Now I have one of Nige's soap testing kits but have never tried or got my head around it as I am useless at colour changes and figure this is a necessity.
Did that other kit I sent ever show up Steve?
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Now I have one of Nige's soap testing kits but have never tried or got my head around it as I am useless at colour changes and figure this is a necessity.
Did that other kit I sent ever show up Steve?
I only ever received the one mate.
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..some theiving gits in the post office >:(
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..some theiving gits in the post office >:(
That is the only package I have ever had go missing, some people are very unlucky with the post office. Having said that I am now getting stuff delivered to my new house and have not forged a relationship with delivery drivers and postman, so who knows what the future may bring ! !
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I've done some tests.
this is a 50/50 test, 250ml of washed bio and 250ml of hot (boiled) water
(http://i250.photobucket.com/albums/gg264/mark405td/003-2.jpg)
this is the same 50/50 with 4 drops of acetone added
(http://i250.photobucket.com/albums/gg264/mark405td/001-2.jpg)
I did a tatrated soap test on both samples,
the first sample had 76ppm of soaps,
the second 36ppm of soaps,
so a drop of 40ppm after adding the acetone, over 50% reduction.
So yes acetone dose help the soaps migrate into the water.
My feelings are it's due to the acetone lowering surface tension as the 50/50 split noteably quicker.
Now who's going to test this with the demeth and settle method.
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Intresting to try on demethed, unwashed and unsettled bio to see if it could possibly replace settling and washing.
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If I can nick my eldest daughters nail Polish remover I'll have a go. Interesting so far. Would a drop of petrol do the same though?
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I can't see that it will replace settling or washing, but may speed things up.
If I'm right and it's the lack of surface tension that's making the difference dose petrol do the same,
I mean we add petrol to thin our bio/veg, but some add acetone to improve combustion, whereas petrol reduces com busion,
so does it have the same effect on surface tension ?
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I've done some tests.
this is a 50/50 test, 250ml of washed bio and 250ml of hot (boiled) water
(http://i250.photobucket.com/albums/gg264/mark405td/003-2.jpg)
this is the same 50/50 with 4 drops of acetone added
(http://i250.photobucket.com/albums/gg264/mark405td/001-2.jpg)
I did a tatrated soap test on both samples,
the first sample had 76ppm of soaps,
the second 36ppm of soaps,
so a drop of 40ppm after adding the acetone, over 50% reduction.
So yes acetone dose help the soaps migrate into the water.
My feelings are it's due to the acetone lowering surface tension as the 50/50 split noteably quicker.
Now who's going to test this with the demeth and settle method.
Thanks Mark, it's nice when an idea works.
I shall add some to my wash water on the next batch and see how much it speeds up the washing process.
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If I'm right and it's the lack of surface tension that's making the difference dose petrol do the same,
I mean we add petrol to thin our bio/veg, but some add acetone to improve combustion, whereas petrol reduces com busion,
so does it have the same effect on surface tension ?
I don't believe Petrol does as adding Acetone to Petrol has the same effect and advantages in a Petrol engine.
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That's sooo cool! Love new discoveries...
Any idea how much we'd need to add to 100 litres for example?
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That's sooo cool! Love new discoveries...
Any idea how much we'd need to add to 100 litres for example?
I reckon I will try about 1% ie: 18ml in my 180Ltr batches.
I think you may be right that it could work as an emulsion breaker too.
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I've done some tests.
this is a 50/50 test, 250ml of washed bio and 250ml of hot (boiled) water
(http://i250.photobucket.com/albums/gg264/mark405td/003-2.jpg)
this is the same 50/50 with 4 drops of acetone added
(http://i250.photobucket.com/albums/gg264/mark405td/001-2.jpg)
I did a tatrated soap test on both samples,
the first sample had 76ppm of soaps,
the second 36ppm of soaps,
so a drop of 40ppm after adding the acetone, over 50% reduction.
So yes acetone dose help the soaps migrate into the water.
My feelings are it's due to the acetone lowering surface tension as the 50/50 split noteably quicker.
Now who's going to test this with the demeth and settle method.
Mark you don't fancy posting your findings on the other side do you ? (as you have the pictures and accurate soap figures)
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After adding the Acetone, water washing and then drying does the bio still look clear? Do you still need to add acetone prior to using it (i.e. does the acetone go with the water layer or stay with the bio)?
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After adding the Acetone, water washing and then drying does the bio still look clear? Do you still need to add acetone prior to using it (i.e. does the acetone go with the water layer or stay with the bio)?
The sample we did the other day has sat on the side here since, the bio on top of the water is now crystal clear. I am guessing here but I think the Acetone left in the Bio will vaporise off during drying.
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I started a batch today and will be washing it over the next two days,
so on the final wash I'll put some acetone in and see how it goes when scaled up,
it should be easy enough to count how many drips make 1ml and calculate the dosage for a full batch.
What are your thoughts on adding it to the second wash as well (I normally do three washes),
I doubt there's any benefit from using it on the first wash with the acid.
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That's sooo cool! Love new discoveries...
Any idea how much we'd need to add to 100 litres for example?
I reckon I will try about 1% ie: 18ml in my 180Ltr batches.
I think you may be right that it could work as an emulsion breaker too.
Steve 1% is 180ml. 18ml is 0.1%.
Acetone as an emulsion breaker, now that's an interesting idea.
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Good result that mark,not tried the acid wash yet .
Cheers
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It's just accrued to me that some have noticed deposits dropping out after adding petrol to there bio,
so maybe there is something in the theory that petrol will help soaps settling after demeth,
if this is what's happening then it also suggests that acetone will be good for demeth and settle.
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Mark you don't fancy posting your findings on the other side do you ? (as you have the pictures and accurate soap figures)
I will once I've done more tests and others have had similar results.
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I don't want to rain on your parade guys but there really is no need to add unnecessary chemicals to your bio to lower the soap ppm's further. As a final wash, try a hot pump wash. The residual heat left behind after this process is then used to dry the bio.
Nige
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I was going to comment on cost of heating vs cost of acetone but I guess if you're water washing you have to heat it anyway to dry it.
So hot water is better at soap extraction than cold water?
What about both for an amazingly clear result?
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Nige, personally I like to do cold washing, I think it helps remove HMPE's.
Also we may be able to reduce the amount of washes required,
unless we test these things we'll never know.
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When you're down to about 10ppm is it really worth adding another step to the process?
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When you're down to about 10ppm is it really worth adding another step to the process?
But if we can get down to 10ppm with less steps (washes) then surely it's worth doing.
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Nige, personally I like to do cold washing, I think it helps remove HMPE's.
Also we may be able to reduce the amount of washes required,
unless we test these things we'll never know.
I do all my washes cold except for the last one which is done at drying temp for me..about 55C. I'm also down to 3-4 washes including the hot pump wash. That works out at 40lts to wash 150lts of bio. I l also think that cold or hot washes will see the end of HMPE's
I didn't mean to have a pop at the testing Mark. That was not my intention. I was, however, suggesting that adding acetone could be seen as unnecessary due to some rather efficient washing methods. It certainly is with the way I process.
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I didn't mean to have a pop at the testing Mark. That was not my intention. I was, however, suggesting that adding acetone could be seen as unnecessary due to some rather efficient washing methods. It certainly is with the way I process.
Not taken as a pop mate.
A balanced viewpoint is always welcome.
Would you mind posting your washing method (as you know I'm a recent convet and have not read to much about water washing in the past).
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It's no big secret or anything new and revolutionary. I use a:
http://www.ebay.co.uk/itm/60-LTR-AIR-PUMP-KOI-PONDS-HYDROPONIC-HAILEA-ACO-318-/200867775989?pt=UK_HomeGarden_Garden_PondsWaterFeatures_UK&hash=item2ec4a705f5
and a 3" ceramic airstone controlled with a 6mm aquarium screw valve. The bubbles for the washes are really gentle for the first 2 washes. The first is genearlly over night and drained off with out being left to stand. Never needed to do that. Another 10lts is then poured in and the pump turned back on again. This is then drained and replaced when I get back from work. For wash 3 the air valve is opened up a bit to allow a bit more aggression and left to bubble over night. By the morning the bio generally has taken on a clear appearance. I let this settle while I'm at work and drain when I get back. I turn the heat on and when up to temperature I bubble on full bore and pump wash with my central heating pump for 30mins or so. Allow to settle and dry with air and a uri geller diffusser.
That's it...no smoke or mirrors here
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So you bubble wash, for some reason I thought you mist washed.
I did bubble wash in my early days, but had enough of going back and forth with buckets of water,
I'm still setup for it now and hope to have running water and drainage in the shed by the summer.
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Nope...never mist washed, always bubbled. I think some make it over complicated with some stages which arn't entirely needed. The issue some have is having the bubbles too aggressive in the early stages. Then bang on about emulsions and never going back to it. Horses and courses I know but gently to begin with is the key to my method
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Nope...never mist washed, always bubbled. I think some make it over complicated with some stages which arn't entirely needed. The issue some have is having the bubbles too aggressive in the early stages. Then bang on about emulsions and never going back to it. Horses and courses I know but gently to begin with is the key to my method
Nige, how long does your process take? How many interventions? I also tried bubbling a long time ago, but so much has changed since. Maybe worth another look?
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Glyc wash, two stage process with ASM 30%, 7% post reaction water wash, 3-4 10lt bubble washes, dry.......that's it.
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Hi mate
Gathered most of that! But post reaction, how long does the process take until you have useable fuel?
Just trying to see if there's something there that might suit me.
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from the start of washing to usable fuel..if I was in a desperate rush would be 36-48hrs. However, I always have fuel in stock and I've never been in a position where I've needed to rush things. I always plan my fuel making well in advance. Rushing fuel production will ultimately lead to errors and mistakes. It ain't a race!
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That's sooo cool! Love new discoveries...
Any idea how much we'd need to add to 100 litres for example?
I reckon I will try about 1% ie: 18ml in my 180Ltr batches.
I think you may be right that it could work as an emulsion breaker too.
Steve 1% is 180ml. 18ml is 0.1%.
Acetone as an emulsion breaker, now that's an interesting idea.
Oooops thanks for pointing that out Mark, I always put the decimal point in the wrong place ! !
I would think that few water washers are getting the amazing results that Nige is (20 to 30% batch size amount of water resulting in 10ppm soap with no HMPE's), for those that are maybe this is unlikely to help in anyway.
As a born again water washer who has not perfected such an easy method I will carry on testing with the next batch I make and report back with any findings I feel are pertinent.
I must say that reading the negative comments to the possibility that this may be a diversification that helps in some way has felt more like reading a thread on VOD rather than on here.
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That's sooo cool! Love new discoveries...
Any idea how much we'd need to add to 100 litres for example?
I reckon I will try about 1% ie: 18ml in my 180Ltr batches.
I think you may be right that it could work as an emulsion breaker too.
Steve 1% is 180ml. 18ml is 0.1%.
Acetone as an emulsion breaker, now that's an interesting idea.
Oooops thanks for pointing that out Mark, I always put the decimal point in the wrong place ! !
I would think that few water washers are getting the amazing results that Nige is (20 to 30% batch size amount of water resulting in 10ppm soap with no HMPE's), for those that are maybe this is unlikely to help in anyway.
As a born again water washer who has not perfected such an easy method I will carry on testing with the next batch I make and report back with any findings I feel are pertinent.
I must say that reading the negative comments to the possibility that this may be a diversification that helps in some way has felt more like reading a thread on VOD rather than on here.
Still in the wrong place, 1% of 180L is 1.8L, 0.1% is 180ml, 0.01% is 18ml
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Hi Steve
I'm happy to try it on my system to see if I can get some positive results that could be posted up and also I can do some tests on the bench with wvo. All up for trying stuff to see what effect it has.
Paul
Do you have enough or should I get some
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That's sooo cool! Love new discoveries...
Any idea how much we'd need to add to 100 litres for example?
I reckon I will try about 1% ie: 18ml in my 180Ltr batches.
I think you may be right that it could work as an emulsion breaker too.
Steve 1% is 180ml. 18ml is 0.1%.
Acetone as an emulsion breaker, now that's an interesting idea.
Oooops thanks for pointing that out Mark, I always put the decimal point in the wrong place ! !
I would think that few water washers are getting the amazing results that Nige is (20 to 30% batch size amount of water resulting in 10ppm soap with no HMPE's), for those that are maybe this is unlikely to help in anyway.
As a born again water washer who has not perfected such an easy method I will carry on testing with the next batch I make and report back with any findings I feel are pertinent.
I must say that reading the negative comments to the possibility that this may be a diversification that helps in some way has felt more like reading a thread on VOD rather than on here.
Still in the wrong place, 1% of 180L is 1.8L, 0.1% is 180ml, 0.01% is 18ml
LOL thanks Richard... luckily I had the amount in my head rather than the calculation ! ! and as it happens that works out at the percentage I originally found out to add in the final fuel way back when ! ! now that is a coincidence.
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I must say that reading the negative comments to the possibility that this may be a diversification that helps in some way has felt more like reading a thread on VOD rather than on here.
My comments Steve were posted as a positive statement not a negative one. As Mark says:
"A balanced viewpoint is always welcome."
The method, dispite being in it's infancy, could well have an impact on soap reductions. Only time and additional testing will prove it off.
For me...I cant see it happening when water washing brings me the kind of results I've posted details of on this thread.
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I must say that reading the negative comments to the possibility that this may be a diversification that helps in some way has felt more like reading a thread on VOD rather than on here.
My comments Steve were posted as a positive statement not a negative one. As Mark says:
"A balanced viewpoint is always welcome."
The method, dispite being in it's infancy, could well have an impact on soap reductions. Only time and additional testing will prove it off.
For me...I cant see it happening when water washing brings me the kind of results I've posted details of on this thread.
Nige this is hardly a positive statement.
"I don't want to rain on your parade guys but there really is no need to add unnecessary chemicals to your bio to lower the soap ppm's further. As a final wash, try a hot pump wash. The residual heat left behind after this process is then used to dry the bio.
Nige"
I wont make anymore references to it.... Promise...
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Positive/negative...it's a position of perspective.
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from the start of washing to usable fuel..if I was in a desperate rush would be 36-48hrs. However, I always have fuel in stock and I've never been in a position where I've needed to rush things. I always plan my fuel making well in advance. Rushing fuel production will ultimately lead to errors and mistakes. It ain't a race!
Nige
No need to defend it... It is what it is! Just wondered if it would work for the way I want to do things.
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from the start of washing to usable fuel..if I was in a desperate rush would be 36-48hrs. However, I always have fuel in stock and I've never been in a position where I've needed to rush things. I always plan my fuel making well in advance. Rushing fuel production will ultimately lead to errors and mistakes. It ain't a race!
Nige
No need to defend it... It is what it is! Just wondered if it would work for the way I want to do things.
Water washing is a very effective way of reducing the soaps to virtually nothing if done correctly...ie gently. Too many people have got into difficulty by rushing and being too aggressive with the bubbles. As I undersand, the titrated acid water wash is extremely effective at removing soaps quickly. Not a method I've adopted yet.
I think the only way it will help with the way you want to things is if you wash gently.
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I've been doing some more tests today (well I've been playing anyway).
Counting drips of acetone it seems that 1ml = 37 drips.
Now working on my previous test I used 4 drips in 250ml of bio,
so 16 drips to 1L,
so 1ml treats as near as dammit 2.25L.
The second wash (with just water) is settling over night, so tomorrow I'll do the third wash with 80ml of acetone added and post the results.
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I must add that the initial dose of 4 drips in 250ml of bio was just a starting point,
we may find that this can be increased/decreased with further testing.
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rather than counting drips i think it would be a lot easier and more accurate to weight it and make an adjustment for the SG. the scales used for titration should be good enough. drips come in different sizes so one persons 4 drips will be different to someone else's 4 drips.
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Thanks Mark for taking the idea on board and testing.
With my original test sample the water side is still very cloudy and has not cleared the way the water does on a normal 50/50 and has fairly large lumpy white bits on the split line . Nathan commented that the Bio seems to be less viscous than normal too !
Maybe this has pulled out HMPE's too or even something that causes waxing, so temperature test's would be good but we would have to compare treated back to back with untreated Bio from the same batch for accurate comparison.
I will be pulling a few litres of Raw bio from my next batch for playing with and will use your drip calculations for treating the full batch, I intend to add it with the first water wash after acid neutralisation.
edited more viscous to less viscous as pointed out by Nathan.
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Nathan commented that the Bio seems to be more viscous than normal too !
Steve, did you mean that it appeared to have a lower viscosity - thinner?
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Mate my brain is going... DUH.... less viscous... thinner... runnier... lol
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Some results for you.
Just before going to bed I decided to add 20ml (1/2 of the intended dose for the last wash) of acetone to the batch (this was the second wash) and put the pump on a timer for 1hr.
This morning I took a sample and did a 50/50 (250ml/250ml), this had a clear slit and clear water,
I added 4 drips of acetone and it stayed clear,
I tested it for soaps with a result of 42.56 :)
To recap
180l batch, two stage non titration, clear 10/90 pass.
titrated acid wash with 30L of water, pumped for 3 hr, settled of 3hr.
second wash with 45l of water, pumped for 2hr, 20ml of acetone added and pumped for a further 1hr,
settled for 12hr, tests done.
The batch is now drying.
I have now run out of IPA so can't do any further tests for a while.
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rather than counting drips i think it would be a lot easier and more accurate to weight it and make an adjustment for the SG. the scales used for titration should be good enough. drips come in different sizes so one persons 4 drips will be different to someone else's 4 drips.
This is why I counted the amount of drips per 1ml and have used ml in my posted calculations, we all have syringes.
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Thanks Mark for taking the idea on board and testing.
With my original test sample the water side is still very cloudy and has not cleared the way the water does on a normal 50/50 and has fairly large lumpy white bits on the split line . Nathan commented that the Bio seems to be less viscous than normal too !
Maybe this has pulled out HMPE's too or even something that causes waxing, so temperature test's would be good but we would have to compare treated back to back with untreated Bio from the same batch for accurate comparison.
I will be pulling a few litres of Raw bio from my next batch for playing with and will use your drip calculations for treating the full batch, I intend to add it with the first water wash after acid neutralisation.
edited more viscous to less viscous as pointed out by Nathan.
I'm happy to do the tests Steve, thanks for posting your ideas.
My first 50/50 with added acetone did partly clear but was not as clear as the 50/50 without the acetone, I had no lumpy white bits on the split line.
Maybe you had more soaps present, or it may just be different feed stock.
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I have now run out of IPA so can't do any further tests for a while.
As we are testing with Acetone hopefully you mean you have run out of that and not IPA lol.
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Some results for you.
Just before going to bed I decided to add 20ml (1/2 of the intended dose for the last wash) of acetone to the batch (this was the second wash) and put the pump on a timer for 1hr.
This morning I took a sample and did a 50/50 (250ml/250ml), this had a clear slit and clear water,
I added 4 drips of acetone and it stayed clear,
I tested it for soaps with a result of 42.56 :)
To recap
180l batch, two stage non titration, clear 10/90 pass.
titrated acid wash with 30L of water, pumped for 3 hr, settled of 3hr.
second wash with 45l of water, pumped for 2hr, 20ml of acetone added and pumped for a further 1hr,
settled for 12hr, tests done.
The batch is now drying.
I have now run out of IPA so can't do any further tests for a while.
So does that mean using the Acetone has completed the job in less washes than it would normally take Mark ?
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I have now run out of IPA so can't do any further tests for a while.
As we are testing with Acetone hopefully you mean you have run out of that and not IPA lol.
IPA is for the soap tests.
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So does that mean using the Acetone has completed the job in less washes than it would normally take Mark ?
Yes, I normally do 3 or 4 washes.
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So does that mean using the Acetone has completed the job in less washes than it would normally take Mark ?
Yes, I normally do 3 or 4 washes.
Wicked, that's a good result for starters. My batch is made, when I get to wash it I will be adding the Acetone with the first wash.
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How much are you going to add ?
I used 20ml in 180L of bio.
I hope your results confirm my findings.
Do you do titrated acid washing, if you do I wouldn't add the acetone to the first wash as we have no idea what the outcome will be,
maybe Carrington can enlighten us on this.
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How much are you going to add ?
I used 20ml in 180L of bio.
I hope your results confirm my findings.
Do you do titrated acid washing, if you do I wouldn't add the acetone to the first wash as we have no idea what the outcome will be,
maybe Carrington can enlighten us on this.
My last one was... but I have demethed this batch as I believe the Methanol interferes with washing too. Sooo.. I will be talking to Paul first. And using an amount along your lines. Cheers Mark.
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but I have demethed this batch as I believe the Methanol interferes with washing too.
I've believe that too! I'm sure that when I've demethed (bit fiddly without a venturi - pulling in air on the suction side of the pump), washing has been easier.
I'd be interested in testing meth % on each wash, but as I've mentioned previously I've a theory that meth ppms or % reduces over successive washes until it reaches a threshold where soaps release at higher volumes. I could be wrong, but everything that I've seen with years of water washing suggest this.
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Any results yet Steve ?
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Hi Mark,
no sorry I have not had a chance to catch up with Paul yet, I did a 50/50 with bio from the bottom and to be honest it was not that white so I have high hopes once I get to neutralise it and give it a wash.
As this batch will have had a fair settling time I will keep a sample before washing and one after to do some side by side cold testing which may be interesting too.
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Side by side testing would be great.
Once I some more IPA I'll do the same.
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Side by side testing would be great.
Once I some more IPA I'll do the same.
What testing are you doing with IPA Mark ?
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Side by side testing would be great.
Once I some more IPA I'll do the same.
What testing are you doing with IPA Mark ?
I rather suspect, Steve, that mark has run out of IPA for performing titrated soap tests. A key ingredient and test for for what you're trying to acheive.
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Side by side testing would be great.
Once I some more IPA I'll do the same.
What testing are you doing with IPA Mark ?
I rather suspect, Steve, that mark has run out of IPA for performing titrated soap tests. A key ingredient and test for for what you're trying to acheive.
Ah I understand now, cheers.
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I've got a batch from a week and a half back that seems to be settling rather slowly, so I've taken a 75ml sample and added 0.5ml Acetone (0.66%)
I'll compare this for soap with the rest of the batch later this week.
I'm also about to make a new batch tomorrow, I was going to take 2x 500ml samples in the same jars, one with and one without acetone to compare settling of those. What percentage do you think I should try?
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Tony, I added 20ml to 180L of bio for my washing,
that works out at around 0.1ml per liter,
this could be a starting point for you.
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That's not much at all. I'll try 0.1ml in each 500ml sample then.
The one that wasn't settling is showing some faint signs of soap at the bottom today.
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I have had a demethed KoH 180 litre batch settling in my reactor for the last week or so, once a day I have been dropping the glyc, all nice and dark.
Yesterday only a drip came out so I put in 200ml of Acetone and mixed for 20 minutes at ambient temp. Today I dropped 350ml of dark glyc ! So it has released more from the Bio. I will see what drops tomorrow and then take a sample for a 50/50 test.
I may end up not washing this batch and the next batch will get the Acetone after demething and probably once it has cooled a bit.
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This is looking all very interesting.
If I ever manage to make bio again, I'll give it a try!
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This is looking all very interesting.
If I ever manage to make bio again, I'll give it a try!
Yes I am glad I tried Acetone and put it out here, I think it could become a player in the process.
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I have had a demethed KoH 180 litre batch settling in my reactor for the last week or so, once a day I have been dropping the glyc, all nice and dark.
Yesterday only a drip came out so I put in 200ml of Acetone and mixed for 20 minutes at ambient temp. Today I dropped 350ml of dark glyc ! So it has released more from the Bio. I will see what drops tomorrow and then take a sample for a 50/50 test.
I may end up not washing this batch and the next batch will get the Acetone after demething and probably once it has cooled a bit.
So are you saying that you can add the acetone & not water wash? Does the acetone have to be removed from the bio?
Many thanks,
Nick.
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That's interesting Steve, it's not going to work for NaOH users but KOH and ASM users may find it usefull.
200ml is quite a lot though, I used just 20ml in my water wash test.
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So are you saying that you can add the acetone & not water wash? Does the acetone have to be removed from the bio?
Many thanks,
Nick.
I've a good feeling that acetone will help with settling after demeth (Tony is doing some testing on this).
Acetone is used by some (manly vey runners) to improove combustion, but only at 0.05% (I think), it has been found to have no benifit in increasing this.
So there should be no need to remove the acetone.
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So are you saying that you can add the acetone & not water wash? Does the acetone have to be removed from the bio?
Many thanks,
Nick.
I've a good feeling that acetone will help with settling after demeth (Tony is doing some testing on this).
Acetone is used by some (manly vey runners) to improove combustion, but only at 0.05% (I think), it has been found to have no benifit in increasing this.
So there should be no need to remove the acetone.
Thank you Mark. Why would it have no effect withNaOH users, and how would the presence of acetone affect an EN14214 test?
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NaOH goes solid in the pipework when cooled, so you can't leave it overnight for more to drop out.
I have no idea about the EN test.
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NaOH goes solid in the pipework when cooled, so you can't leave it overnight for more to drop out.
I have no idea about the EN test.
It could be added before it goes to the settling tank,after demeth, though, that may cause faster/ more compleat settling.
Dick
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NaOH goes solid in the pipework when cooled, so you can't leave it overnight for more to drop out.
I have no idea about the EN test.
It could be added before it goes to the settling tank,after demeth, though, that may cause faster/ more compleat settling.
Dick
This is what Tony is testing at pressent.
Hopefully he'll post some info soon.
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I have been chatting to Jerry (CHUNDER on the other site) tonight,
he uses 50ml of acetone + 6l of petrol + recamended dose of vegyboost in 60L of oil (veg runner).
He has doorstop samples and has noticed that ones with acetone added hold on to the fats,
whereas the ones without drop the fats.
Both cloud as the temp drops but the acetone one still holds the fats.
So it seams that acetone has many uses in our little hobby.
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That's interesting Steve, it's not going to work for NaOH users but KOH and ASM users may find it usefull.
200ml is quite a lot though, I used just 20ml in my water wash test.
Not understanding why it wont work for NaOH users !
If it encourages more glyc to initially drop then there will be less if any that could set in the pipework, and ASM is Sodium too so also sets.
I will see what drops tomorrow, have a mix up and take a sample to do a 50/50 test.
The next batch will get 150ml but it will go in as soon as the temperature of the Bio has dropped after demeth, then I will see how the glyc drops over the following days.
I cant decide whether to wash this batch or not at the moment. I think first I want to cool it further and fuge it.
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.
He has doorstop samples and has noticed that ones with acetone added hold on to the fats,
whereas the ones without drop the fats.
Both cloud as the temp drops but the acetone one still holds the fats.
So it seams that acetone has many uses in our little hobby.
That must be a good thing for veg users, the last thing they want is fats dropping in the tank.
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[/quote]
ASM is Sodium too so also sets.
[/quote]
That's the main reason that I went back to KOH. It's sometimes useful to just leave to settle for a few days, rather than feel rushed to stay around until the glyc has properly dropped.
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I am not sure how long acetone would stay in solution of bio that is settling/being bubbled. It is quite volatile so will evaporate.
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I agree, adding it during hot bubbling would probably make no difference as it'd get driven off.
I've done a batch, bubbled and then taken two samples (then at ambient temp), one of which has acetone in for comparison purposes. It looks clear and golden so it'll be interesting to see the lighter soaps drop out over time.
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I put a couple of hundred ml of acetone (all I had left in a 5 litre can) in the first water wash of my two stage, no titration, in processor water washed batch yesterday. 300 litre batch.
First wash was the acid one, 500ml of concentrated Sulphuric acid in 25litres of water.
After that drained off, the second was the acetone, mixed with 45 litres of water, washed and settled for 3hrs then drained.
The water looked very contraminated but the bio was quite light in colour.
I did a second water wash with 45 litres of water and no acetone, mixed for 20mins then left it to settle overnight.
This morning the water was crystal clear so I drained it and started spray drying the bio which was sparklingly clear in three hours.
I suspect that, as Mark found, the Acetone really helped the first water wash leaving much less contamination in the bio for the second wash to take out.
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I've just done my second batch using the acetone wash,
1st wash was the acid wash, 20l water and 400ml of hydrochloric acid (estimated due to lack of IPA)
2nd was with 30L of water and 40mm of acetone (twice the amount of acetone I used last time just to see if it made any difference),
50/50 is crystal clear, I can't do a titrated soap test as I have no IPA left.
I'm going to post these results on the VOD so all can benefit from our findings.
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All good results with Acetone on the washing front and also looking good on using Acetone in the reaction too which if washed after I am thinking it will be even more straight forward. At the moment I am playing with settling though.
Well done the testers. Good stuff.
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I've just done my second batch using the acetone wash,
1st wash was the acid wash, 20l water and 400ml of hydrochloric acid (estimated due to lack of IPA)
2nd was with 30L of water and 40mm of acetone (twice the amount of acetone I used last time just to see if it made any difference),
50/50 is crystal clear, I can't do a titrated soap test as I have no IPA left.
I'm going to post these results on the VOD so all can benefit from our findings.
Mark..with all due respect you have no results. You have changed your methods but as yet have no results. Without checking for soaps in a before and after test you have nothing to compare your results against. We all know how unreliable a 50/50 test is (me more than most with the testing I did a couple of years ago). It needs some proper testing to back up any findings you come across.
Nige
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I've just done my second batch using the acetone wash,
1st wash was the acid wash, 20l water and 400ml of hydrochloric acid (estimated due to lack of IPA)
2nd was with 30L of water and 40mm of acetone (twice the amount of acetone I used last time just to see if it made any difference),
50/50 is crystal clear, I can't do a titrated soap test as I have no IPA left.
I'm going to post these results on the VOD so all can benefit from our findings.
Mark..with all due respect you have no results. You have changed your methods but as yet have no results. Without checking for soaps in a before and after test you have nothing to compare your results against. We all know how unreliable a 50/50 test is (me more than most with the testing I did a couple of years ago). It needs some proper testing to back up any findings you come across.
Nige
I think he does have results, he used to take 4 to 5 washes to get a clear 50/50..... now its 2 washes so that must be an improvement... final soap amounts in PPM's will require your test !
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Nige, I know I haven't done any side by side testing so it's not scientific,
however previous batches with the same feed stock have needed 3 or 4 washes (not counting the acid wash) to get down to around 50ppm soap,
allthough 50/50 tests are not accurate form your own admition a clear test indicates a ppm of less than 100 (I think that's what you quoted, correct me if I'm wrong).
As most bio producers don't do titrated soap tests and rely on 50/50 alone, they should benefit from this method.
To get a clear 50/50 after just one pumped water wash is, I believe, a good result.
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I don't think I've ever made that statement about 50/50 tests Mark. Far too vague. If I have I would like to retract it. If you can find it anywhere let me know and I'll edit it.
Steve...doing something once could be seen a something of fluke. It really needs to be backed up with data over many batches including PPM results to have any sort of credability. Only then can it be seen as a result.
I hope it's not a fluke and proves to be beneficial to Marks fuel production...indeed to anyones fuel. I'm trying to give my comments some sort of scientific credence. A 50/50 test is far from that. The PPM data is important here. Mark has a kit...you have a kit. Mark has the equipment to have backed up the claim.
......and Yes I understand the importance of the claim of 4-5 washes down to 2.
Nige
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I don't think I've ever made that statement about 50/50 tests Mark. Far too vague. If I have I would like to retract it. If you can find it anywhere let me know and I'll edit it.
Steve...doing something once could be seen a something of fluke. It really needs to be backed up with data over many batches including PPM results to have any sort of credability. Only then can it be seen as a result.
I hope it's not a fluke and proves to be beneficial to Marks fuel production...indeed to anyones fuel. I'm trying to give my comments some sort of scientific credence. A 50/50 test is far from that. The PPM data is important here. Mark has a kit...you have a kit. Mark has the equipment to have backed up the claim.
......and Yes I understand the importance of the claim of 4-5 washes down to 2.
Nige
Okay Nige.
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I don't think I've ever made that statement about 50/50 tests Mark. Far too vague. If I have I would like to retract it. If you can find it anywhere let me know and I'll edit it.
Steve...doing something once could be seen a something of fluke. It really needs to be backed up with data over many batches including PPM results to have any sort of credability. Only then can it be seen as a result.
I hope it's not a fluke and proves to be beneficial to Marks fuel production...indeed to anyones fuel. I'm trying to give my comments some sort of scientific credence. A 50/50 test is far from that. The PPM data is important here. Mark has a kit...you have a kit. Mark has the equipment to have backed up the claim.
......and Yes I understand the importance of the claim of 4-5 washes down to 2.
Nige
Yes Nige I have a kit, but correct me if I am wrong here but it's accuracy depends upon colour change and my eye as to when and how much that colour change has happened would have no accuracy at all.
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I don't think I've ever made that statement about 50/50 tests Mark. Far too vague. If I have I would like to retract it. If you can find it anywhere let me know and I'll edit it.
Steve...doing something once could be seen a something of fluke. It really needs to be backed up with data over many batches including PPM results to have any sort of credability. Only then can it be seen as a result.
I hope it's not a fluke and proves to be beneficial to Marks fuel production...indeed to anyones fuel. I'm trying to give my comments some sort of scientific credence. A 50/50 test is far from that. The PPM data is important here. Mark has a kit...you have a kit. Mark has the equipment to have backed up the claim.
......and Yes I understand the importance of the claim of 4-5 washes down to 2.
Nige
Yes Nige I have a kit, but correct me if I am wrong here but it's accuracy depends upon colour change and my eye as to when and how much that colour change has happened would have no accuracy at all.
Which was one of the failings of feedstock titration method.
My view for what it's worth is that those who are seeking out progress are bright enough to add rigour as they go. One of the attractions of this site is that it is, and has the opportunity to remain collaborative, where VOD has gone the opposite way. So rather than be negative, get involved, share your results or stand on the sidelines!
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Who's being negative Nathan?
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That is rather unfortunate Steve...not being able to detect a colour change in the test kit. It does make it a tad redundant. Probably best to pass it on to someone who can benefit from. If you wish, I could undertake some tests for you, FOC, if that helps. Let me know and I'll send you my address.
Nige
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Who's being negative Nathan?
I don't want to rain on your parade guys but there really is no need to add unnecessary chemicals to your bio to lower the soap ppm's further. As a final wash, try a hot pump wash. The residual heat left behind after this process is then used to dry the bio.
Nige
I've just done my second batch using the acetone wash,
1st wash was the acid wash, 20l water and 400ml of hydrochloric acid (estimated due to lack of IPA)
2nd was with 30L of water and 40mm of acetone (twice the amount of acetone I used last time just to see if it made any difference),
50/50 is crystal clear, I can't do a titrated soap test as I have no IPA left.
I'm going to post these results on the VOD so all can benefit from our findings.
Mark..with all due respect you have no results. You have changed your methods but as yet have no results. Without checking for soaps in a before and after test you have nothing to compare your results against. We all know how unreliable a 50/50 test is (me more than most with the testing I did a couple of years ago). It needs some proper testing to back up any findings you come across.
Nige
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Since when has it been negative to point out the flaws in a test program?
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Since when has it been negative to point out the flaws in a test program?
I refer u to my previous comments
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is there any other way to test for soaps that doesn't involve a colour change? looking at a sample under a microscope for instance. laser reflection spectroscopy? none of these need be expensive.
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If by your" comments" you mean "my quotes" then I stand by those as two very positve statements.
You don't need to add additional chemicals to a water wash process in order to lower the ppm's. Very positive statement
Recordable data over several batches is the bare minimum required in order to prove off a process. Another very positive statement.
Where is the negativity above?
Nige
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So anyway Steve / Mark do you think the acetone stays with the bio layer, meaning that no further acetone is require for the finished fuel (ie remain in solution)?? Would it flash off through the spray bar? Are there any inexpensive test methods?
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I don't think I've ever made that statement about 50/50 tests Mark. Far too vague. If I have I would like to retract it. If you can find it anywhere let me know and I'll edit it.
Nige
Nige,
I, like most of us, do a lot of reading on here and the VOD,
I'm sure I've read something in that vain and thought it was posted by you.
Out of interest, and I know you've done a good amount of testing on this, what would you say a clear 50/50 test indicates as far as ppm levels.
I know I have tested one of mine at 76ppm.
I do appreciate your comments, and don't see them as negative, more of an independent view.
I can sometimes get carried away with my enthusiasm.
When I do my next batch, if I have time and some more IPA, I'll remove half the batch after the acid wash stage and do some back to back tests, standard pump washing V's acetone washing, doing titrated soap test along the way.
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So anyway Steve / Mark do you think the acetone stays with the bio layer, meaning that no further acetone is require for the finished fuel (ie remain in solution)?? Would it flash off through the spray bar? Are there any inexpensive test methods?
I would have thought it evaporates off in the drying stage, or in my method anyway.
I take the bio up to 95C and condense off the remaining water, then pump it into the drying/storage tank and bubble overnight.
Hopefully when I build my next setup (on hold at pressent, due to funds) I'll have a heater in the drying tank so I can setup a defuser or spray bar and reduce the temps.
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Well at least you're still talking to me Mark:)
Nathan...pick up your dummy. :'(
Mark. I wouldn't like to guess as to what levels of soap in PPM's are in a clear 50/50. Following my testing using water gathered from different parts of the country it is ultimately down to the water quality of that particular area.
Thankyou for your comments about my independant views. ;)
Further to your last statement I would do a soap test after every stage to see how far they have been reduced. If you need more chemicalsin order to complete the testing let me know and I'll send some down FOC
Nige
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If by your" comments" you mean "my quotes" then I stand by those as two very positve statements.
You don't need to add additional chemicals to a water wash process in order to lower the ppm's. Very positive statement
Recordable data over several batches is the bare minimum required in order to prove off a process. Another very positive statement.
Where is the negativity above?
Nige
Nige I don't recall anyone saying using Acetone reduces the soap levels below that of water washing.
What it has shown to do is make the soap drop quicker and more complete seriously reducing the amount of washes needed.
And it's interactions with the reaction process are even more amazing.
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The implication...made by me...is that the reduction of soaps by use of acetone is a "speed"related process. This may or may not be the case, but only postive test results will prove it off. My view is that with careful washing via the bubble method will get you to low PPM's if done efficiently without the need for further intervention
Nige
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Well at least you're still talking to me Mark:)
Nathan...pick up your dummy. :'(
Mark. I wouldn't like to guess as to what levels of soap in PPM's are in a clear 50/50. Following my testing using water gathered from different parts of the country it is ultimately down to the water quality of that particular area.
Thankyou for your comments about my independant views. ;)
Further to your last statement I would do a soap test after every stage to see how far they have been reduced. If you need more chemicalsin order to complete the testing let me know and I'll send some down FOC
Nige
Nige. I'm pretty easy going and it takes a lot to pee me off, you're nowhere close as yet mate ;)
As I've stated before, this forum only works to push things forward if we all add our thoughts and findings.
A wold of "yes men" would not progress in any way.
I do actually admire you, you're not afraid to post what I'm sure you realise may be taken as negative.
As far as chemicals goes I'll be putting in an order to Basic for some more meths, so I'll add IPA to that.
Thanks for the offer though.
In interests of moving forward, would you like to do some testing with acetone and bubble washing ?
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Has anyone seen this?
http://pubs.rsc.org/en/Content/ArticleLanding/2011/GC/c1gc15049a (http://pubs.rsc.org/en/Content/ArticleLanding/2011/GC/c1gc15049a)
Don't know if it is relevant to the discussion. Haven't bought the full pdf.
If its not relevant just ignore me :)
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Yes photoman bought it I think, it is being looked at!
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just been reading this thread and its very interesting, would love to try this myself maybe as i both water wash and sometimes pump wash
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I've had some promissing results so Far,
it would be great to see if you find it beneficial also.
Do you have one of Nige's soap test kits ?
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Mark..I think some people need to lay off tagging posts as negative. These are just different views which some don't like. A statement is a statement. The inference of negativity is often maligned and misunderstood. As previously stated, it's a matter of perspective.
The offer of chemicals did not extend to IPA I'm afraid. I was infering the acid and Bromophenol blue. If you need any more of these during your testing then please let me know. No charge.
Glenn...if you don't have a kit let me know. In the interest of testing I'll send a kit to you FOC.
I'm not sure I want to get involved with testing. Purely for the reason that my methods really suit me at the moment. I've not even got involved with the acid water washing which has proved to be a huge leap forward in home brewing. I'm not sure I want to add unnecessary chemicals to my fuel in order to speed up the removal of soap. I've almost completed my batch from Saturday with 4 x 10lt washes on a 150lt. No additional chems used.
Nige
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Nige. I have plenty of acid and Bromophenol blue left (still not half way through the first bottles).
But I could do with another 0.5ml syringe as I knocked it off the side and stood on it today while having a tidy up (a rare thing in my shed).
Once we've got the acetone pump washing down to a tee I'll do some bubble wash testing.
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Send me you addy via the message service and I'll pop a couple in the post.
Nige
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Mark, if you're over this way I've got loads of IPA if you want some.
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Mark..I think some people need to lay off tagging posts as negative. These are just different views which some don't like. A statement is a statement. The inference of negativity is often maligned and misunderstood. As previously stated, it's a matter of perspective.
Nige
My last say on this. (thank goodness I hear some say)
This thread is in the interest of further development that can and has lead to even more developments and interesting reaction processes using Acetone..
Your early post of and I quote :
"I don't want to rain on your parade guys but there really is no need to add unnecessary chemicals to your bio to lower the soap ppm's further. As a final wash, try a hot pump wash. The residual heat left behind after this process is then used to dry the bio.
Nige"
We never said that it was to lower the soap ppm's further so it is Negative or of no use with regard to the thread and has no place what so ever in the thread because it is nothing to do with adding Acetone or the benefits of it.
If your View as you put it was you are not interested, your process is perfect as it is and you have no interest in testing then why did you bother to " rain on our parade" because we are interested or we would not be trying things outside the box.
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Send me you addy via the message service and I'll pop a couple in the post.
Nige
PM sent.
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Come on guy's, it's getting like the VOD.
Lets get back on track and keep going with the job in hand.
One of the best things about the wiki forum is it's openness and lack of bickering.
Nige has made his position clear, he's got a process that works for him, he has in the past helped many others produce low soap fuel (myself included).
He's even put a test kit together and offers it to other members at a very reasonable price.
So he is working with us, not against us.
Steve is working towards pushing acetone reactions forward, and from what I've read, so far it's looking very promising.
I've done some testing with acetion in the wash water, others seam to want to take up the testing on this also.
Julian and others have done testing on on adding acid to the reaction before demething.
The acid pump washing is now getting widely used.
So, we're all working together, for a common goal of pushing things forward.
So lets sit back, take a deep breath and remember what we're trying to do.
We have made great gains in a short time, all of this has been done through the cooperation of members.
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well said mark we need results good ones and failures, especially the failures. that is how the process will progress. having a water jacketed processor is definatley the safer option with acetone recovery. i now a bit more about cold traps than i did, still not enough. keep finding all the stuff on acetone recovery seems to geared towards illegal substance extraction. will try and wade though it. given the sort of people wanting to know how its done ,wading is definatly the correct term. man..... bet they are all 14 and from somewhere in Arizona.
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Mark..I think some people need to lay off tagging posts as negative. These are just different views which some don't like. A statement is a statement. The inference of negativity is often maligned and misunderstood. As previously stated, it's a matter of perspective.
Nige
My last say on this. (thank goodness I hear some say)
This thread is in the interest of further development that can and has lead to even more developments and interesting reaction processes using Acetone..
Your early post of and I quote :
"I don't want to rain on your parade guys but there really is no need to add unnecessary chemicals to your bio to lower the soap ppm's further. As a final wash, try a hot pump wash. The residual heat left behind after this process is then used to dry the bio.
Nige"
We never said that it was to lower the soap ppm's further so it is Negative or of no use with regard to the thread and has no place what so ever in the thread because it is nothing to do with adding Acetone or the benefits of it.
If your View as you put it was you are not interested, your process is perfect as it is and you have no interest in testing then why did you bother to " rain on our parade" because we are interested or we would not be trying things outside the box.
I was merely trying to enlighten you to the possibilities of washing effectivly, efficiently and without the need for additional chemicals. All my comments have been positive and I have a process that you might want to exam at some point. I remember a few years ago when water washing was considered wasteful and old fashioned and the future lay at the door of WBD. We all know which direction that's going. The future is sometimes to be found in the past. I think I'll put that in my sig 8)
I will always post up my positive comments where I feel the less experinced would benefit and discuss them accordingly.
Thank goodness you've had your last say ;)
Mark..VOD or no VOD this is a discussion forum.
I hope that your soaps are SETTLED to your satisfaction at a speed you are happy with. I know mine are. ;D
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Results are in:
- two 500ml samples from a batch that has had the Methanol bubbled off
- 0.1ml Acetone put in one sample
- settled for 9 days
Both have a similar layer of light soap at the bottom, and a soap test indicates very similar soap content, so Acetone for settling alone does not appear to help at this concentration.
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Tanks Tony, this test has been usefull,
but may have been more usefull it's soap tests were to have been done on each day rather than at the end.
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what would you say a clear 50/50 test indicates as far as ppm levels.
I know I have tested one of mine at 76ppm.
I still do 50/50 tests as it's quicker and easier than Nige's soap test (though the buck stops at the titrated test for accuracy).
The trouble is that "clear" water covers a range of ppms soap, probably up to 100ppm even before it begins to look less sparkly. This is where lasers come in, in a dark room a laser through the water layer will show a beam right down to the lower ppms. If I can't make out the beam in a dark room I reckon it's down at <25ppm (though I've not done any formal testing on this - might be worth experimenting!). I always use near boiling water to get quick and clean separation. I feel that the 50/50 still has a place in testing but it's very much one of those things that takes a while to get a feel for, rather than the titrated test which is consistent every time.
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I agree the 50/50 test still has a use, I have, and still do, use fuel that passes this test.
However when we are doing testing/researching of new methods this should only be used as an indication that soap content is starting to drop to titrated testing levels.
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Results are in:
- two 500ml samples from a batch that has had the Methanol bubbled off
- 0.1ml Acetone put in one sample
- settled for 9 days
Both have a similar layer of light soap at the bottom, and a soap test indicates very similar soap content, so Acetone for settling alone does not appear to help at this concentration.
Is there any reason Tony for testing at 9 days. How did you come up with this as a time frame?
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So, we're all working together, for a common goal of pushing things forward.
So lets sit back, take a deep breath and remember what we're trying to do.
We have made great gains in a short time, all of this has been done through the cooperation of members.
Well said Mark.
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Results are in:
- two 500ml samples from a batch that has had the Methanol bubbled off
- 0.1ml Acetone put in one sample
- settled for 9 days
Both have a similar layer of light soap at the bottom, and a soap test indicates very similar soap content, so Acetone for settling alone does not appear to help at this concentration.
Is there any reason Tony for testing at 9 days. How did you come up with this as a time frame?
A great many reasons, none of which relate to scientific rigour but do relate to daughter's 13th birthday party, snow, cancellation of party, being bloody cold and having more fun indoors battling the lad with Nerf guns in the warm :)
OK so usually my winter process involves settling for two weeks, this test is therefore somewhat towards the end but I wanted some soap still present in the control sample for the test - in case with the Acetone it had all dropped like a stone leaving me with miraculously clear biodiesel, which doesn't appear the case. Sure I could test every day all the way through, but have you been out there? Brrr!
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I remember a few years ago when water washing was considered wasteful and old fashioned and the future lay at the door of WBD. We all know which direction that's going.
What, you're not still using water are you grandpa? ;D
The future is sometimes to be found in the past. I think I'll put that in my sig 8)
Totally agree, WBD and settle all the way! No water in my process thankyou very much ;)
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what would you say a clear 50/50 test indicates as far as ppm levels.
I know I have tested one of mine at 76ppm.
I still do 50/50 tests as it's quicker and easier than Nige's soap test (though the buck stops at the titrated test for accuracy).
The trouble is that "clear" water covers a range of ppms soap, probably up to 100ppm even before it begins to look less sparkly. This is where lasers come in, in a dark room a laser through the water layer will show a beam right down to the lower ppms. If I can't make out the beam in a dark room I reckon it's down at <25ppm (though I've not done any formal testing on this - might be worth experimenting!). I always use near boiling water to get quick and clean separation. I feel that the 50/50 still has a place in testing but it's very much one of those things that takes a while to get a feel for, rather than the titrated test which is consistent every time.
in the days when you could still get scientific instruments for next to nothing i had a thing called a specker. very simple device.
it had 2 photcells back to back in the middle and 2 lights at the ends of a tube. there are 2 holes in the tube equal distances apart from the centre. you put a test tube with a standard solution, in our case clean water. in one hole and the solution under test in the other. soapy water in this case. turn on the lights and read the difference in voltage on the photocells. quick and easy to do with 2 cheap multimeters. or you could make it as complex as you wanted to with go no go leds or something. you would need to balance it first with 2 test tubes of the standard solution to compensate for any differences in the photocells.
the key thing is the principle. its straight out of john strong if anyone remembers his column in scientific american. it can be used for much more complex than just soap detection by using different refractive index solutions and different types of glass but should work fine for a simple soap test. if you where very clever you could make up a soap test kit with the correct colour index and use that as a standard. would need to establish the standard first of course. nigel could do that has he has most experience of the test he could then send out test tubes with a standard colour. not sure how long it would stay the same colour though. maybe some permanent dye the right colour would be better.
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I used to work for a company that designed Diesel smoke testers for MOT. Light at one end of tube, photocell at other end, you had some "calibration smoke" (actually a special darkened glass to insert into the tube) then you could go ahead and test using exhaust smoke. The hard bit was stability of the optics over time and keeping them clean. Very similar principles.
Particle counters use laser backscatter, no reason why we can't do the same with a laser pen and judge by eye :)
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ah but has steve has pointed out eyes vary. :o
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So we are saying that a 50/50 can give a positive (clear) result at over double the ASTM?
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As an aside does anybody object if I change "the three" to four on the soap page? As I feel water can do as much if not more damage
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Which page is that Keith?
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I think he means the top of the soap test page.
I'd say yes, go ahead and perhaps qualify it further by saying ..."one of the four main" ...
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Results are in:
- two 500ml samples from a batch that has had the Methanol bubbled off
- 0.1ml Acetone put in one sample
- settled for 9 days
Both have a similar layer of light soap at the bottom, and a soap test indicates very similar soap content, so Acetone for settling alone does not appear to help at this concentration.
Just a thought Tony, if you still have them would you try adding say, 200ml water to each as they are, shake the hell out of them to get the soap back in and settle to see what happens, then if the water is a different colour soap test the Bio again.
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The future is sometimes to be found in the past. I think I'll put that in my sig 8)
Totally agree, WBD and settle all the way! No water in my process thankyou very much ;)
.......just HMPE's and days upon days of waiting ;D
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I've made a start on an acetone wash page,
it's by no means compleat as yet, or in the right format (I've tried but got confused).
Please take a look and feel free to edit so it's in the right format.
http://www.biopowered.co.uk/wiki/Using_acetone_to_aid_soap_removal
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Good start, but I can see you're thinking forum code ... you need to think wiki code! Just a few simple bits of markup which can be copied from any wiki page or from one of the stickies on the forum.
If it's OK with you I'll start another thread to guide you through the page, in the hope that it will be useful to others too.
Did you start by copying and pasting from the "New Page", page?
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Yes I started by copy/past the "new page", but got lost soon after.
Please do start a new thread to guide me through, I need help.
I'm fine with spanners, electrics, pipework, anything with my hands really, but this is using my head, and that's allways been the weak point.
Edit to say my spelling is also a weak point (before anyone else said it).
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Just had a look at the page and it reads well.
Good work mark I know who to send my findings to on new test for the write ups
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The future is sometimes to be found in the past. I think I'll put that in my sig 8)
Totally agree, WBD and settle all the way! No water in my process thankyou very much ;)
.......just HMPE's and days upon days of waiting ;D
I'll see your multiple water washes and raise you playing with the kids in the warm while it gets on with it on it's own while the recovered Methanol sits there waiting for the next batch ;)
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I've made a start on an acetone wash page,
it's by no means compleat as yet, or in the right format (I've tried but got confused).
Please take a look and feel free to edit so it's in the right format.
http://www.biopowered.co.uk/wiki/Using_acetone_to_aid_soap_removal
Easily understood (the most important bit about portraying information), the rest is just prettying up which it sounds like Julian would like to encourage you to learn - but failing that just a bit of formatting from a few wiki old hands* and that's perfect :)
*personally I can never remember wiki formatting and have to crib from existing pages every time!
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*personally I can never remember wiki formatting and have to crib from existing pages every time!
I'm exactly the same.
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well just ordered some acetone to try on my next batch :) :)
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Mark,
I have just edited your page to make it look as, I expect, you wanted it to.
Good write up and pictures mate (which I have not changed at all other than the spelling mistakes which I noticed as I went along). Feel free to add extra text in there.
I have also put the links in to other pages and indexed it on the main page so finding you work is now easier for others. It is in the 'finishing' section of 'biodiesel'
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Mark,
I have just edited your page to make it look as, I expect, you wanted it to.
Good write up and pictures mate (which I have not changed at all). Feel free to add extra text in there.
Thanks Jules, shall I delete this thread I put together for Mark, then?
http://www.biopowered.co.uk/forum/index.php/topic,900.0.html
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Sorry mate - maybe I should have read that :-[
Not well today and day off from work so, sitting down with nothing to do and the laptop in front of me it seemed helpful.
At least what I have done matches very well with your instructions to Mark and, hopefully, passes your scrutiny.
Once again, my apologies
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Sorry mate - maybe I should have read that :-[
Not well today and day off from work so, sitting down with nothing to do and the laptop in front of me it seemed helpful.
At least what I have done matches very well with your instructions to Mark and, hopefully, passes your scrutiny.
Once again, my apologies
It's OK, I was just trying to help Mark get his head round wiking, perhaps another time. Or if you really want a bash at it, Mark, we could roll the page back.
It's not really up to me to scrutinise or pass anything, it's all a joint effort ... I just made some suggestions, hope it didn't sound too dictatorial!
Sorry to hear your feeling unwell, but if your twiddling your thumbs, your Glogs page needs finishing ... I'm dying to know how to store these things.
Also I did make some comments on the ASM page, don't know if you saw them. Is it worth adding that titration is done with 1% NaOH solution and changing the formula to read ml instead of grams? Both points confused me when I followed it to use ASM (but then confusing me is not a difficult thing to do).
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No problem. I think it is good that you and Tony are quite specific on how wiki pages should be, that is what keeps the uniformity.
I have made your suggestions to the ASM page now. I hope it looks better.
I will have a bash at the glogs page soon.
I just store them stacked up in what used to be a coal bunker and is now lined with a tarpaulin. The only downside I have found to that is that by the time I have used a couple of hundred, the bottom ones are quite damp. I believe this is down to glycerol being hygroscopic and absorbing moisture from the air.
They still burn OK but need a bit more heat to get going and there is an audible crackling and popping from the water
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No problem. I think it is good that you and Tony are quite specific on how wiki pages should be, that is what keeps the uniformity.
I have made your suggestions to the ASM page now. I hope it looks better.
I will have a bash at the glogs page soon.
I just store them stacked up in what used to be a coal bunker and is now lined with a tarpaulin. The only downside I have found to that is that by the time I have used a couple of hundred, the bottom ones are quite damp. I believe this is down to glycerol being hygroscopic and absorbing moisture from the air.
They still burn OK but need a bit more heat to get going and there is an audible crackling and popping from the water
did my sawdust contact work out ok jules? the stuff you had off me had been sitting around for at least a year maybe 2. it is green when they cut it so there will be a lot of water in it before you make the glogs,plus they spray the saw to keep the dust down.
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Glogs page now updated and looking better too
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Glogs page now updated and looking better too
Looking great!
I took a picture of some carpet cores a while back and forgot to upload it (done now)
(http://www.biopowered.co.uk/w/images/5/57/Packing_tape_closing_one_end_of_a_Glog_tube.JPG)
I find putting tape across one end helps when you come to pack the sawdust. I tend to only use one piece now though.
Anyhow if it's of use please feel free to use it. I'm going to fill some TetraPaks in the next few days, so if photos of that in progress would help let me know.
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Ideal, I will put that one in. Pics of the process would be good I think, I meant to take some last time I make some logs but forgot.
........ Do you think we may have gone a bit off topic here?
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Jules, thanks for fixing the page, good job some one knows what they're doing.
I will make some changes once I've done a few more batches,
I plan to do a batch and split it in two, standard pump washing one half,
and acetone washing the other,
I'll do titrated soap tests at every wash stage.
This should give some good comparison results for the page.
But it may be about a month before I can get it done though, unless I get chance to pop over to Julian for some IPA.
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No problem, you are very welcome.
You are doing the hard work, I just made it look pretty
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........ Do you think we may have gone a bit off topic here?
That's what topics are for.
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... unless I get chance to pop over to Julian for some IPA.
Offer's still there. I should be in most of the week but possibly out Friday.
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... unless I get chance to pop over to Julian for some IPA.
Offer's still there. I should be in most of the week but possibly out Friday.
I'm not off work until Sunday, I'll see she'll let me out to play.
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I started my next test today.
I'll add all the info on here so I can reference it when I update the wiki page.
200L batch
Glycerol prewash
Two stage non titration
1st stage 25L methanol and 800g of NaOH
2.5ml dropout in 90/10 test
2nd stage 7L methanol and 240g of NaOH
clear pass 90/10
Glycerol drained
450ml of hydrochloric acid added to 20L of water, pumped for 1hr.
settled for 3hrs, water drained
190L left in reactor
95L (half the batch) drained into clean containers.
50ml sample taken (will test for soap content before washing).
15% water added (without acetone) pump washed for 1hr.
The idea is to do standard pump washes on half the batch and do a soap test after each wash,
once that's done, dried and in the settling/storage tank I'll acetone wash and soap test the other half,
this will give a good compareson test between the two washing methods.
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Sounds good Mark.
Nice to see some Biodiesel experimentation going on these days, keeps it interesting :)
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Bio has become interesting again with the advent of two stage non titration, titrated acid washing and more recently the developments in the use of acetone.
The fun has returned.
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Bio has become interesting again with the advent of two stage non titration, titrated acid washing and more recently the developments in the use of acetone.
The fun has returned.
Nice one Mark, I have to take a forced period off from playing, had carpal tunnel done on my left hand last week (right was done in Dec) , half the wound is open and infected ! ! ! going to take a while to sort itself Doc say's today. I need to give it a fighting chance so really must refrain till it's mended. Grrrrrrrrrrrrrrrrrrrrrrr
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nice one mark, would love to get my pump washing down to just a couple of washes.
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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.
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Bio has become interesting again with the advent of two stage non titration, titrated acid washing and more recently the developments in the use of acetone.
The fun has returned.
Nice one Mark, I have to take a forced period off from playing, had carpal tunnel done on my left hand last week (right was done in Dec) , half the wound is open and infected ! ! ! going to take a while to sort itself Doc say's today. I need to give it a fighting chance so really must refrain till it's mended. Grrrrrrrrrrrrrrrrrrrrrrr
Sounds painfull mate, but stay away from the bio until it's healed up properly, I know it's going to be hard though.
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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?
-
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?
No, this is the batch I'm doing a compareson test with,
half the batch is being washed without acetone and the other half with acetone,
the idea was to do titrated soap tests at all stages to prove the advantage of acetone.
But so far is not working.
I have however just done a 50/50 test on the unwashed half and it's cloudy.
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.
-
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.
-
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.
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Mark....you have a personal message regarding the questions you posed.
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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.
-
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.
-
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.
-
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.
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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.
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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.
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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.
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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.
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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.
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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.
-
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.
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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.
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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.
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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.
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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.
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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.
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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
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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
Paul, that seems in line with what I said, or did I miss something?
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Sorry Nathan I just read the last post by Jim when I posted
You got it
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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
So I was right in thinking that the titrated soap test is effected by the acid wash, as it works on PH value.
This will be why my soap tests have shown low ppm even on the unwashed sample.
So the only soap test that will truly show accurate results is the 50/50 test (which isn't accurate) >:(
I know I can use a Lazar pen but this still doesn't produce a quantifiable figure.
I'll just have to do my next batch without the acid wash so I can get accurate results for the "use of acetone to remove soaps" page.
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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
Come on Mark spit it out lad !
Edited, please read again.
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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
So I was right in thinking that the titrated soap test is effected by the acid wash, as it works on PH value.
This will be why my soap tests have shown low ppm even on the unwashed sample.
So the only soap test that will truly show accurate results is the 50/50 test (which isn't accurate) >:(
I know I can use a Lazar pen but this still doesn't produce a quantifiable figure.
I'll just have to do my next batch without the acid wash so I can get accurate results for the "use of acetone to remove soaps" page.
The way I see it is using acid has simply reduced extra soap production in the first place. Your tests still show whether using Acetone gets the soaps out quicker, all be it less of them so still very helpful and a good comparison.
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I agree it still shows good results from the method, but they're not quantifiable.
Doing it without the acid wash will be, also it'll be good to prove the method works without the acid wash,
showing it's more versatile.
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I've just finished my second 100ltr batch using Acid and Acetone, this time I added 2ml/ltr to the first Titrated Acid (80ml H2SO4) wash water.
1st wash was 10ltr run for 1hr and settled over night.
2nd wash just 10ltr of water washed fro 30mins and settled for a couple of hours.
A 50/50 soap test after the second wash showed crystal clear water, I gave it a 3rd wash just to make sure though, it's now drying in the reactor using the condenser and water is flowing nicely at only 60°C, y'can beat a squirrel for rapid evaporation.
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I've just finished my second 100ltr batch using Acid and Acetone, this time I added 2ml/ltr to the first Titrated Acid (80ml H2SO4) wash water.
1st wash was 10ltr run for 1hr and settled over night.
2nd wash just 10ltr of water washed fro 30mins and settled for a couple of hours.
A 50/50 soap test after the second wash showed crystal clear water, I gave it a 3rd wash just to make sure though, it's now drying in the reactor using the condenser and water is flowing nicely at only 60°C, y'can beat a squirrel for rapid evaporation.
It certainly does seem to have at least halved the washing that used to be required, are you finding reduced HMPE's now your washing Jim ?
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so you added 2ml per litre of acetone with the first acid wash..correct or did you do an acid wash first then add the acetone in with the second wash... just to be clear here.. :)
got my asm now so cant wait to do my forst batch..
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[quote author=1958steveflying link=topic=860.msg9474#msg9474 date=1360529840
It certainly does seem to have at least halved the washing that used to be required, are you finding reduced HMPE's now your washing Jim ?
[/quote]
I can't really comment of the reduction of washes as these last two batches are the first I've ever washed.
As for HMPE's I haven't really suffered since I've been using the titless method with ASM, I've had the odd batch with a few but nothing serious.
Glenn, yes I did add 2ml/ltr to the first acid wash water, worked for me.
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So... what du think? will you continue with the water?
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So... what du think? will you continue with the water?
Mmmmmmmmmmm! To be honest I think it's a complete PITA, what used to take me less than an hour hands on over one evening now takes a two days and a lot more intervention and power.
The only advantage I can see is if you can devote the time over a weekend you'll have fuel for Monday morning as against having to wait several days for settlement.
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So... what du think? will you continue with the water?
Mmmmmmmmmmm! To be honest I think it's a complete PITA, what used to take me less than an hour hands on over one evening now takes a two days and a lot more intervention and power.
The only advantage I can see is if you can devote the time over a weekend you'll have fuel for Monday morning as against having to wait several days for settlement.
Fair comment!
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That's really good news Jim, both you and Jules have had similar results to me.
This has spurred me on to get the next batch done once my meths gets here,
it's semi solid wet gunk that will need drying before the gly wash,
so should be a good test batch with interesting results.
I know it's no good for this time of year but I need to get some of my collection drums emptied.
Once it's done I'll pump into a 220L drum ready for the warmer weather.
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I have finished another batch, it wasn't a full batch semi solid wet gunk but around 25%, 75% good liquid oil.
I had problems with the reaction and had to do a third stage to get a good pass (oil not as dry as it could have been)
this meant there was more methanol left in the bio and higher amounts of soap produced.
It was acid washed (I knew this batch was not going to be good for test results), then an acetone wash.
The acetone wash did not work as well as previous batches, and the washwater still smelt of meths.
So looking back at the other batches that were non titration two stage with 16% meths, I think it's more effective when methanol and soap levels are reasonably low.
This I think is backed up by the results Julian had recently.
I'm going to try demething before washing as I think this will help with soap removal.
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I'm going to try demething before washing as I think this will help with soap removal.
I've demethed both batches before the acid wash phase and the wash water still had a slight whiff of methanol.
For my last batch I returned to demeth bubble and settle but this time I added 15ml of acetone to the 100ltr of bio once it hit approx 20C, continued bubbling for 30mins and settled.
The idea was to see if the soaps settled faster, they seemed to but the result is somewhat subjective.
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The general concensus is that most of the soaps will not wash out until most of the meths has been removed,
this is why I want to demeth before washing.
Tony also tried using acetone when settling, but he didn't see any benefit to it.
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With Julians recent results I use acetone on this batch but carried on with a couple of washes afterwards,
50/50 tests showed that not all the soap was removed and I ended up doing 5 washes.
I have no soap test results due to getting my samples mixed up (I should have marked them) and having to do an acid wash due to an emulsion.
My next batch will be using ASM, hopefully tomorrow.