Dis ASM, he mighty pow'ful magic! (or ... have I witnessed a reverse reaction)

[Julian]

Following on from this thread ... http://www.biopowered.co.uk/forum/index.php/topic,865.msg7685.html#msg7685

There's something really screwy going on.

The bio had sat in the processor and cooled to 26°C over night.  I took a sample and it looked reasonable, a few soapy lumps but OK.  I decided to play it safe and just add winteriser, pump out and settle.  This seemed to have worked for all the samples I'd taken.

So I did just that.  Quite nice looking bio pumped into the settling tank, then suddenly I got thick, grayish/brown soap.  Pumping out from the bottom of the tank means that all this gunge was floating on the bio.  Even I know hat's just not what's supposed to happen.

I stopped the pump quickly, drained the remnants into a barrel and spent the rest of the day trying to work out what was going on.  I could well be wrong, but I'm pretty dammed sure the oil was dry.  If that was the case there's no water present to make soap.  Added to that the soap appeared at the demeth stage not the reaction stage.

To my knowledge in four years of reading bio forums, although is often talked about, no one has ever claimed to have one or described what a reverse reaction looks like.  With no chemistry knowledge you would assume if would revert to oil, but what if that wasn't the case and it reverts/converts to some other gloop?

Could what I'm seeing be the elusive reverse reaction.  It upholds my claim the oil was dry. It appeared at the right time in the process.  It appeared after a long demeth period. It could explain the strange floating behaviour of the "soap" and the rubbery glycerol which set in the pipe work within an hour.

I did cock up on the sums, but only a little and what I gained by my error I lost by reducing the base , so not massively overdosed with catalyst.

Ducks and waits for incoming!

[nathanrobo]

Hypothetical, but based on something said by a guy with a warwick uni degree in chemistry & supported by another ex-chemist.  You have a triglyceride, you pull off or chop off it's three fatty acids, leaving a glyc molecule with 3 entry points.  Then you remove meth, leaving alkanes & glyc.  Under the right conditions the glyc re-attaches fatty acids, giving mono, Di & triglycerides.

Kinda good theory... True???

[Carrington]

Hi Julian
Have you tested the gunge with 90/10 test to see if it converted , also if you do a 50/50 test it might show you if there is much catylist left or if its been spent converting your bio back to oil.

I would expect any material that has been re-converted to settle lower then the bio as this would have the heavy glycerine attached but I could be wrong.

Another test would be to mix some water and acid give it a mix in sample jar and leave to settle to see if it stays gloppy or turns back to nice bio.

I'm lookin forward to seeing how this goes.

Paul

[julianf]

If there was reverse reaction, i would have thought that the triglyceride would disolve in the remaining methylester?

What i mean is that you mention pumping out some 'good' product, before the 'stuff'.  Assuming the 'good' stuff was methylester, whatever the other bit did not seem soluable in it?

[Julian]

Hi Julian
Have you tested the gunge with 90/10 test to see if it converted , also if you do a 50/50 test it might show you if there is much catylist left or if its been spent converting your bio back to oil.

I would expect any material that has been re-converted to settle lower then the bio as this would have the heavy glycerine attached but I could be wrong.

Another test would be to mix some water and acid give it a mix in sample jar and leave to settle to see if it stays gloppy or turns back to nice bio.

I'm lookin forward to seeing how this goes.

Paul

I'll give those tests a go in the next couple of days and post the results.  What should I be looking for in each case?

[nigelb]

This is rather interesting but at the same time really unfortunate. I'm confident that it's nothing to do with the ASM or there would have been other users posting up on both forums.

I hope you find a solution to what's going on Julian but I'm not going to have a guess as to what it is. Not a scooby doo I'm afraid.

[Julian]

So far I've recovered around 60+ litres from what should have been 80.  I'll probably squeeze a bit more from the drained soap or what ever it is.

First batch I've not washed in a long time and it can only have seen a minimum of say 7-8°C and I get this when I pump out of the settling tank - HMPE central ...

[Julian]

Second ASM batch today ... yet another miserable failure!

Soap, soap and yet more soap right from adding the ASM this time, so not quite as unusual as the last batch.

I dewatered for several hours using the compressor, at 95°C this time and got out about ½ a litre of water out of 80 litres.  Stupidly I didn't do a HPT.

Again I went for a titrated two stage, replicating what I always do making the only change the catalyst.

80 litre batch, titrating at 4.5ml  and I used a base of 3.5ml/l which gave me 3.2 litres of ASM and I used 12.6 litres of Methanol.

I'd added about ¾ of the first stage when I noticed a sample starting to gel.

I tried adding more methanol which reduced/delayed the gelling but after adding 4 litres it still wasn't behaving.

I've tried adding 7% water to a sample as per the wiki and get a beautiful creamy emulsion which shows no signs of breaking.  Maybe needs more Methanol, but I felt nearly an extra 20% should have worked.

In true Carrington style I tried adding a few drops of 1% H₂SO₄ to a sample, not 'cos I know what I'm doing but 'cos I had nothing to loose ... that is showing signs of separating slightly.

Due to the timing of the soaps appearance the most likely cause is wet oil.  I'm wondering if pumping ambient air through the processor in these damp conditions could be the cause.

Also can another ASM user confirm that this stuff is meant have a considerably higher viscosity than Methanol?

Any suggestions on attempts to recover 80 litres of soap welcomed!

[1958steveflying]

Second ASM batch today ... yet another miserable failure!

Soap, soap and yet more soap right from adding the ASM this time, so not quite as unusual as the last batch.

I dewatered for several hours using the compressor, at 95°C this time and got out about ½ a litre of water out of 80 litres.  Stupidly I didn't do a HPT.

Again I went for a titrated two stage, replicating what I always do making the only change the catalyst.

80 litre batch, titrating at 4.5ml  and I used a base of 3.5ml/l which gave me 3.2 litres of ASM and I used 12.6 litres of Methanol.

I'd added about ¾ of the first stage when I noticed a sample starting to gel.

I tried adding more methanol which reduced/delayed the gelling but after adding 4 litres it still wasn't behaving.

I've tried adding 7% water to a sample as per the wiki and get a beautiful creamy emulsion which shows no signs of breaking.  Maybe needs more Methanol, but I felt nearly an extra 20% should have worked.

In true Carrington style I tried adding a few drops of 1% H₂SO₄ to a sample, not 'cos I know what I'm doing but 'cos I had nothing to loose ... that is showing signs of separating slightly.

Due to the timing of the soaps appearance the most likely cause is wet oil.  I'm wondering if pumping ambient air through the processor in these damp conditions could be the cause.

Also can another ASM user confirm that this stuff is meant have a considerably higher viscosity than Methanol?

Any suggestions on attempts to recover 80 litres of soap welcomed!

If you were doing a no titration 2 stage your 1st stage would be in the region of 1.6 litre's ASM... I can only think the titration part of the process is where it is going wrong.

[Julian]

That's possible.  4.5 is quite high for the oil I normally collect.  So I titrated twice with different supplies of IPA and I did a blank titration both occasions (I don't normally bother).

I could still have made a boo boo but I can't see where.

[1958steveflying]

That's possible.  4.5 is quite high for the oil I normally collect.  So I titrated twice with different supplies of IPA and I did a blank titration both occasions (I don't normally bother).

I could still have made a boo boo but I can't see where.

  Just go with the no titration method and start with 4 X 5 X batch size.

[Julian]

I may have to.  Tried it before and it was a pain in the bottom compaired to two stage titrated.  My methoxide mixer makes the two stage titration method very easy.

Obviously it'll be easier with ASM ... I need to make a decent ASM dispenser anyway.

[photoman290]

i dont the answer, but i suspect the compressor isn't helping. this might help.

http://en.wikipedia.org/wiki/Relative_humidity

there is a chart about half way down that gives the figures. you might well be  filling your oil with water. if it is anything like here, the RH in the coach first thing in the morning is around 70%. it might be worth while gettng a cheap RH meter. mine came with a lidls weather station and was about 12 quid.

[nigelb]

In answer to your question Julian I can confirm that ASM is considerably more viscous than methanol.

I wish I could help in your quest Julian. It is all rather strange. I would re-visit the the no titration method though. I've no idea what my oil titrates at now, it's of no real interest, but I only use on average 3.5lts of ASM to complete a 150lt batch. My batch on Saturday was 2.8 and 0.8

Nige

[Julian]

i dont the answer, but i suspect the compressor isn't helping. this might help.

http://en.wikipedia.org/wiki/Relative_humidity

there is a chart about half way down that gives the figures. you might well be  filling your oil with water. if it is anything like here, the RH in the coach first thing in the morning is around 70%. it might be worth while gettng a cheap RH meter. mine came with a lidls weather station and was about 12 quid.

87% in the South East according to this ...

http://www.eldoradocountyweather.com/forecast/UK-Ireland-Currents/uk-current-relative-humidity.html

So that could be the problem ... just wish I'd done a HPT!