Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: Oilybloke on January 29, 2013, 05:00:09 PM
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Weird, isn't it? I have always used KOH but decided to give the ASM a try. I was amazed at how well it worked, less meth, etc., etc. But, every batch was very heavy with soaps that refuse to settle out. My last two batches have been two stage KOH, soap free, good enough to use after a couple of days settling. Must be the air over here...............
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Hi nick
What base amount did you use as ASM should produce less soap
Paul
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Must be Pilot error, NEVER had a soapy batch with the wonder liquid.
Nick you should be using a base of 3.5 - 4 x 5 x litres first stage and no more than 4 x 5 x litres second stage.
As a matter of interest what is/was your average titration value.
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Thanks for your replies........
I have been using these sums: http://www.biopowered.co.uk/wiki/Anhydrous_sodium_methylate#A_real_world_example
My oil is generally very good quality (mainly GM Soya), used to titrate at 2-3. I have done five batches now, always thoroughly dried, first stage giving 85-95% conversion. The last 3 batches I have not added the glyc for WBD, but demethed by bringing up to 110c and circulating overnight @ 70c., then into settling tank for 5 days. Samples taken from the top for 50/50 are soapy as hell, with HMPEs floating on top and sticking to the sides of the tanks.
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Must be Pilot error, NEVER had a soapy batch with the wonder liquid.
Nick you should be using a base of 3.5 - 4 x 5 x litres first stage and no more than 4 x 5 x litres second stage.
As a matter of interest what is/was your average titration value.
Do you think that it's because I don't have a squirrel?
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No,a squirrel wont make any difference, it just makes demething quicker.
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No,a squirrel wont make any difference, it just makes demething quicker.
Thank you Mark, but I had just asked Jim about a squirrel for my new processor, so a bit of a private joke really......should have added LOL, but just can't bring myself to use text-speak!
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, but demethed by bringing up to 110c and circulating overnight @ 70c.,
I'm not sure I understand what you're saying, are you demething via a condenser? If not how do you know how much meth is left in the bio.
You're probably aware that meth in bio = suspended soap, methanol stops soap particles coalescing and dropping out.
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I've tried three batch with AMS and had little success, I think most likely down to my process ... I'll post more later on the thread concerned. I intend to percivere, though as I can see it has numerous advantages, even at its current price.
I believe the problems were due to water, but all the same I have a feeling the base of five, although Jules states it can be tweaked, is too high. In playing with Dr Pepper tests and the other full size batches, despite them going wrong, I think the maximum base should be reduced to a maximum of 4 with a recommendation people try 3.5 and see how they get on.
Others seem to be using similar figures. How does this fit in with the calculations you did, Jim? While pondering this is it necessary to adjust your formula to account for alternative concentrations of ASM. Most supplies here seem to be 30% at the moment, but others may happen along and anyone overseas using this catalyst may obtain different concentrations.
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Thanks for your replies........
I have been using these sums: http://www.biopowered.co.uk/wiki/Anhydrous_sodium_methylate#A_real_world_example
My oil is generally very good quality (mainly GM Soya), used to titrate at 2-3. I have done five batches now, always thoroughly dried, first stage giving 85-95% conversion. The last 3 batches I have not added the glyc for WBD, but demethed by bringing up to 110c and circulating overnight @ 70c., then into settling tank for 5 days. Samples taken from the top for 50/50 are soapy as hell, with HMPEs floating on top and sticking to the sides of the tanks.
Just a thought but could some of the issues be related to the elevated temps used in the demeth. How much methanol did you recover?
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, but demethed by bringing up to 110c and circulating overnight @ 70c.,
I'm not sure I understand what you're saying, are you demething via a condenser? If not how do you know how much meth is left in the bio.
You're probably aware that meth in bio = suspended soap, methanol stops soap particles coalescing and dropping out.
Yes Jim, de-mething with condenser. Some recent discussions with Nathan showed that I had not been giving enough attention to de-meth (and hence the squirrel enquiry).
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Thanks for your replies........
I have been using these sums: http://www.biopowered.co.uk/wiki/Anhydrous_sodium_methylate#A_real_world_example
My oil is generally very good quality (mainly GM Soya), used to titrate at 2-3. I have done five batches now, always thoroughly dried, first stage giving 85-95% conversion. The last 3 batches I have not added the glyc for WBD, but demethed by bringing up to 110c and circulating overnight @ 70c., then into settling tank for 5 days. Samples taken from the top for 50/50 are soapy as hell, with HMPEs floating on top and sticking to the sides of the tanks.
Just a thought but could some of the issues be related to the elevated temps used in the demeth. How much methanol did you recover?
Recovering about 8 litres from each batch (without the glyc).
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Is that what you would normally expect?
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Two staging with KOH using 36 litres of meth, I would recover 12-14 litres from WBD.
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Thanks for your replies........
I have been using these sums: http://www.biopowered.co.uk/wiki/Anhydrous_sodium_methylate#A_real_world_example
My oil is generally very good quality (mainly GM Soya), used to titrate at 2-3. I have done five batches now, always thoroughly dried, first stage giving 85-95% conversion. The last 3 batches I have not added the glyc for WBD, but demethed by bringing up to 110c and circulating overnight @ 70c., then into settling tank for 5 days. Samples taken from the top for 50/50 are soapy as hell, with HMPEs floating on top and sticking to the sides of the tanks.
Just a thought but could some of the issues be related to the elevated temps used in the demeth. How much methanol did you recover?
Recovering about 8 litres from each batch (without the glyc).
What batch size ? Or have I missed that !
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Oops! No, that's me, 180 litre, Alastair's old processor.
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Hi nick
When is the best time to call you tomorrow
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Any time Paul, do you still have my number?
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I've tried three batch with AMS and had little success, I think most likely down to my process ... I'll post more later on the thread concerned. I intend to percivere, though as I can see it has numerous advantages, even at its current price.
I believe the problems were due to water, but all the same I have a feeling the base of five, although Jules states it can be tweaked, is too high. In playing with Dr Pepper tests and the other full size batches, despite them going wrong, I think the maximum base should be reduced to a maximum of 4 with a recommendation people try 3.5 and see how they get on.
Others seem to be using similar figures. How does this fit in with the calculations you did, Jim? While pondering this is it necessary to adjust your formula to account for alternative concentrations of ASM. Most supplies here seem to be 30% at the moment, but others may happen along and anyone overseas using this catalyst may obtain different concentrations.
The base is 4.0 (as a starting value). The 'magic' number is 5
Therefore it is 5 (magic number) * 4 (or thereabouts - base figure) * litres.
If you used 5 as the base and the magic number then that will explain a lot of problems.
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That's not what the wiki page says, it sates the following:
...A good starting point for the base figure is 5.0 although clearly the base figure is adjustable and can be tweaked to get as low as possible...
However I only used a base of five on the first of the three bathes and that worked, but for much 'soap' manifesting itself at the end of demeth.
I used a base of 4 on the second batch. That went breasts up after only half of the first stage ASM, most likely due to water.
Third batch has proven to be OK despite my panicking, when I used a base of 3.5.
Hence the suggestion that the base on the wiki be reduced.
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That's not what the wiki page says, it sates the following:
...A good starting point for the base figure is 5.0 although clearly the base figure is adjustable and can be tweaked to get as low as possible...
However I only used a base of five on the first of the three bathes and that worked, but for much 'soap' manifesting itself at the end of demeth.
I used a base of 4 on the second batch. That went breasts up after only half of the first stage ASM, most likely due to water.
Third batch has proven to be OK despite my panicking, when I used a base of 3.5.
Hence the suggestion that the base on the wiki be reduced.
Julian your first batch you said had 2700ml of ASM, that works out to a base of 6.75 on an 80 litre batch.
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I'm sure if your oil is dry then you can reduce the base lower. I was using 3.5 and getting less than 10% dropout after stage 1. Reduced it to 3 and still got just 10% dropout, with the same quality oil. Easy stage 2 pass with both base amounts.May try 2.75 next batch.
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I'm sure if your oil is dry then you can reduce the base lower. I was using 3.5 and getting less than 10% dropout after stage 1. Reduced it to 3 and still got just 10% dropout, with the same quality oil. Easy stage 2 pass with both base amounts.May try 2.75 next batch.
I dare say that's down to a quality glyc wash and a bloody good pump. Very impressive figures Rich.
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That's not what the wiki page says, it sates the following:
...A good starting point for the base figure is 5.0 although clearly the base figure is adjustable and can be tweaked to get as low as possible...
However I only used a base of five on the first of the three bathes and that worked, but for much 'soap' manifesting itself at the end of demeth.
I used a base of 4 on the second batch. That went breasts up after only half of the first stage ASM, most likely due to water.
Third batch has proven to be OK despite my panicking, when I used a base of 3.5.
Hence the suggestion that the base on the wiki be reduced.
Julian your first batch you said had 2700ml of ASM, that works out to a base of 6.75 on an 80 litre batch.
I was doing a titrated, two stage batch, so the titrated value was added to the base.
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I'm sure if your oil is dry then you can reduce the base lower. I was using 3.5 and getting less than 10% dropout after stage 1. Reduced it to 3 and still got just 10% dropout, with the same quality oil. Easy stage 2 pass with both base amounts.May try 2.75 next batch.
I dare say that's down to a quality glyc wash and a bloody good pump. Very impressive figures Rich.
Surely the more you reduce the base, the less catalyst there'll be in the glycerine?
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..and those figures go along way in showing the benefits of the No Tit method and the failings of titrations. Strange isn't it that with both methods running side by side the catalyst usage is huge in one and quite skinny in the other
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I'm sure if your oil is dry then you can reduce the base lower. I was using 3.5 and getting less than 10% dropout after stage 1. Reduced it to 3 and still got just 10% dropout, with the same quality oil. Easy stage 2 pass with both base amounts.May try 2.75 next batch.
I dare say that's down to a quality glyc wash and a bloody good pump. Very impressive figures Rich.
Surely the more you reduce the base, the less catalyst there'll be in the glycerine?
Yep, that would be right. Do you see any issue with that?
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I'm sure if your oil is dry then you can reduce the base lower. I was using 3.5 and getting less than 10% dropout after stage 1. Reduced it to 3 and still got just 10% dropout, with the same quality oil. Easy stage 2 pass with both base amounts.May try 2.75 next batch.
I dare say that's down to a quality glyc wash and a bloody good pump. Very impressive figures Rich.
Surely the more you reduce the base, the less catalyst there'll be in the glycerine?
Yep, that would be right. Do you see any issue with that?
Reducing the catalyst is prime, but won't it make the glycerine wash progressively less effective to the point of not being worth the effort?
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Isn't the main benefit the oil drying and the reduction second? or will it be affected?
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Agree with Keith, as getting the oil as dry as possible will have the knock on effect of requiring less catalyst for the conversion.
Since starting with ASM, the amount of glyc that I've got has reduced in line with the reduction in base amount, I used to get out a bit less than the amount of meth used when using NaOH, now, it's way less.
160ltrs of oil in and dried using the venturi, vented to atmosphere, glyc wash, then 24-25lts meth total. Glyc out is now around 16 ltrs.
I also get an increase in the bio out, around 170 after washing.
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Very impressive! I've never Glycerine washed, with my set up reheating the Glycerine would be a real pain, so I'm probably biased.
Now you're using reduced ASM with increased yields, have you considered two identical batches one with and one without Glycerine wash to see if it still has a beneficial effect?
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Reducing the catalyst is prime, but won't it make the glycerine wash progressively less effective to the point of not being worth the effort?
To be honest Julian the primary reason for me havin a glyc wash as part of the process is to have any water/moisture migrate to the glyc. Any transfer of chemicals the other way is a bonus. Having bone dry oil is always worth the effort.
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Very impressive! I've never Glycerine washed, with my set up reheating the Glycerine would be a real pain, so I'm probably biased.
Now you're using reduced ASM with increased yields, have you considered two identical batches one with and one without Glycerine wash to see if it still has a beneficial effect?
Reheating the glycerine for me is a real pain. I heat it up on the turk while the oil is warming up but the benefit is huge.
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Reducing the catalyst is prime, but won't it make the glycerine wash progressively less effective to the point of not being worth the effort?
To be honest Julian the primary reason for me havin a glyc wash as part of the process is to have any water/moisture migrate to the glyc. Any transfer of chemicals the other way is a bonus. Having bone dry oil is always worth the effort.
That's the bit I struggle to get my head round. You can dry the oil conventionally and do a HPT or use a TT (Tosser Tester) to confirm it's dry. After that is there any point in drying further?
Or you could partially dry and Glycerine wash to remove the balance, but you could never be sure just how dry it is.
Were there ever any tests done to quantify the drying effect of a Glycerine wash?
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use a TT (Tosser Tester) to confirm it's dry.
Errr could you enlighten me on what that is? Not sure if I should ask :o
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You must excuse him, he suffers from tourettes!
http://www.biopowered.co.uk/wiki/Water_in_fuel_-_test_kit
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Confusingly this is another TT a Tosser Tube ... http://www.biopowered.co.uk/wiki/Melting_stick
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Very impressive! I've never Glycerine washed, with my set up reheating the Glycerine would be a real pain, so I'm probably biased.
Now you're using reduced ASM with increased yields, have you considered two identical batches one with and one without Glycerine wash to see if it still has a beneficial effect?
I can do that but won't be for some time, as I won't need to brew again for at least a month. Maybe next batch I'll just dry with venturi and not glyc wash. The oil is pretty consistent quality so it shouldn't matter too much of the time difference.
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I think the result would be interesting. Perhaps wait until you've reduced the catalyst as much as you can.
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You must excuse him, he suffers from tourettes!
http://www.biopowered.co.uk/wiki/Water_in_fuel_-_test_kit
Cool thanks think I will make one of those wont annoy the wife with a hot pan test then ;D
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You must excuse him, he suffers from tourettes!
http://www.biopowered.co.uk/wiki/Water_in_fuel_-_test_kit
Cool thanks think I will make one of those wont annoy the wife with a hot pan test then ;D
I know what you mean about wives and HPTs!
A little while ago I bought a cheap solder pot to see if that would work. It worked reasonably well, but the heating element is around the circumference and not on the bottom as I'd expected, and it's supposed to be adjustable down to 100°C, but I measured the temperature at 400°C!
It's in bits to see if it can be modified to run at a lower temperature ... I'm guessing adding a resister may do it but my electronics skills have reached their limit.
I'll get some photos up in a new post and see if any one an help with the modifications.
This the type of thing I bought ... http://www.ebay.co.uk/itm/Round-Stainless-Steel-Solder-Pot-Tin-Furnace-AC-220V-/300825156759?pt=UK_Home_Garden_PowerTools_SM&hash=item460a939c97
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I know what you mean about wives and HPTs!
A little while ago I bought a cheap solder pot to see if that would work. It worked reasonably well, but the heating element is around the circumference and not on the bottom as I'd expected, and it's supposed to be adjustable down to 100°C, but I measured the temperature at 400°C!
It's in bits to see if it can be modified to run at a lower temperature ... I'm guessing adding a resister may do it but my electronics skills have reached their limit.
I'll get some photos up in a new post and see if any one an help with the modifications.
This the type of thing I bought ... http://www.ebay.co.uk/itm/Round-Stainless-Steel-Solder-Pot-Tin-Furnace-AC-220V-/300825156759?pt=UK_Home_Garden_PowerTools_SM&hash=item460a939c97
That looks interesting but I like something I can use that is maybe a bit more quantifiable.
The TT :) means I can have a scale to give an idea of amount of water content based on the reaction. I have done some research and Calcium carbide doesn't react with Acetone or methanol either so was looking at this as a way of testing the distilled acetone/methanol mix for water content, from there it may be possible to weigh the a/m mix and work out the volumes.
One thing I would add to the TT is a pressure relief valve, the section that said
Do not use on a liquid that is obviously wet,i have taken mine above 80psi and when it reaches its limit the gas escapes from the threaded cap BUT there is a danger it could explode at high pressures
HYDROGEN a highly explosive gas is made using this kit
scared me :o The gas that is given off is actually Acetylene not Hydrogen. Calcium carbide is what they used to use for vintage car lamps.
Trouble is I cant really start making things till April as I have just had my bicep tendon re-attached. Hence why I am reading and thinking to much :-\
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Just covering my arse with the exploding bit, there was a cycle valve fitted to release the pressure although I found something posher for Nathans, it works better with calcium hydride but as it is hard to source I left it out (that is what is used in the sandy brae kit)
It could really do with a small airtight metal container but I have yet to find one
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The equipment I use uses calcium hydride and Its expensive. I have been wondering about going over to the carbide when I run out which will be soon
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Just covering my arse with the exploding bit, there was a cycle valve fitted to release the pressure although I found something posher for Nathans, it works better with calcium hydride but as it is hard to source I left it out (that is what is used in the sandy brae kit)
It could really do with a small airtight metal container but I have yet to find one
Its a good design to make at home :)
Calcium carbide giving off acetylene rather than Calcium hydride giving off hydrogen might make it a bit safer? :-\
Do you think it would not be as accurate then?
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, but demethed by bringing up to 110c and circulating overnight @ 70c.,
I'm not sure I understand what you're saying, are you demething via a condenser? If not how do you know how much meth is left in the bio.
You're probably aware that meth in bio = suspended soap, methanol stops soap particles coalescing and dropping out.
Yes Jim, de-mething with condenser. Some recent discussions with Nathan showed that I had not been giving enough attention to de-meth (and hence the squirrel enquiry).
Jim, I have lost your email address, and would like some more details on the squirrel set up. Some pictures perhaps?
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Just covering my arse with the exploding bit, there was a cycle valve fitted to release the pressure although I found something posher for Nathans, it works better with calcium hydride but as it is hard to source I left it out (that is what is used in the sandy brae kit)
It could really do with a small airtight metal container but I have yet to find one
Its a good design to make at home :)
Calcium carbide giving off acetylene rather than Calcium hydride giving off hydrogen might make it a bit safer? :-\
Do you think it would not be as accurate then?
Should be as accurate, its just grinding up the carbide that is time consuming and you get a quicker reaction with the hydride