Biopowered - vegetable oil and biodiesel forum
Biodiesel => Chemistry and process => Topic started by: Julian on December 30, 2012, 10:44:49 PM
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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!
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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???
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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
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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?
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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?
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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.
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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 ...
(http://www.palmergroup.co.uk/Bio/Methacid hmpes.JPG)
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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!
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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.
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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.
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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.
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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.
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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.
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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
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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!
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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
Think I'll have to revisit no titration. But if it's a wet oil issue I'll still have problems! Think I'll have to go back to basics and Dr Peppers to find out what the problem is.
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Nige, your figures match mine well.
I normally use around 7litres of ASM for 300 litres.
6 litres on first stage and around 0.6 to 1.2 on second stage.
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Jules, while you're on line ... the wiki page (quoting JRL) uses grams in the formula for titration amount and base amount. Should these be ml rater than g?
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I'm a great fan (& a recent convert) of no-tit ASM. I use the julesandtash sums from the wiki page and have had great conversions......a couple of other issues, but these are being ironed out (tugs forlock & doffs cap to Nathan). Why titrate when the actual success of the reaction can be simply & accurately measured, and remedied? It seems a lot less hassle and measuring to me....
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So am I the only idiot trying to use ASM with titration?
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So am I the only idiot trying to use ASM with titration?
Mate your the only person using such high quantities of ASM, and I know compressor air is not dry but as a compressor needs water draining from the air receiver I assume it is drier than it goes in. Personally I don't think its a wet oil problem in this instance.
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Third batch with ASM today and yet another batch of gel
Just to recap on the last failure ... to those advocating that non-titration would solve the problem ... the amount of ASM put into the processor was just about equal to what the first stage of a non-titration process would have used ie 1.6 ltrs.
For interest I titrated the oil twice, with different IPA and blank titrated on both occasions ... results 2.0 ml and 2.2ml.
Yesterday I dried the oil taking it to 104°C for nearly an hour, dewatering via the venturi and condenser only. Dewatering was started at around 50°C and continued for an hour or so after the heater was switched off.
Did a HPT which was fine. So I'm starting with indisputably very dry oil.
I took a sample from the processor and ran a non-titration Dr pepper. Did two stages, produced biodiesel and glycerin with no signs of gel. Still had fall out after the second stage, but I'd proved that bio can be created albeit on a very small scale.
For the Dr pepper and the main batch, I used the ASM/Methanol mix left over from the previous batch. I estimated/calculated that this still contained around 1.5/6 ltrs of ASM, so I topped up with Methanol and used that.
The sum I used for the ASM quantity in the first stage was, for an 80 ltr batch, ...
4 (base) X 80 (batch) X 5 (magical constant) = 1.6 ltrs. As the oil titrated at an average of 2.1, this should be nowhere near overdosing.
Today I got as far as adding around half of this, so 800 ml of ASM, when the whole batch gelled. Not as bad as the last, but none the less jelly.
I added 6 ltrs Methanol which made it less vicious, but it was still showing a propensity to solidify when cold.
So ...
Not wet oil.
Not over dosed with ASM.
Not excessively used oil.
Anyone any ideas, 'cos I'm stumped.
These are samples to date ...
(http://www.palmergroup.co.uk/Bio/ASM batch 3 samples.JPG)
From left to right ...
1) Neat sample
2) 50/50 wash test (vigorously shaken, cold water)
3) 50/50 wash test (gently turned end over end, cold water)
4) 50/50 wash test with 10 ml 1% H2SO4 added (vigorously shaken, cold water)
5) 50/50 mix with Methanol (vigorously shaken) ... interesting that the Methanol has seperated.
(http://www.palmergroup.co.uk/Bio/ASM batch 3 Dr Pepper.JPG)
Dr Pepper test, same oil, same catalyst. (sorry, photo a bit dark!)
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Third batch with ASM today and yet another batch of gele.
For the Dr pepper and the main batch, I used the ASM/Methanol mix left over from the previous batch. I estimated/calculated that this still contained around 1.5/6 ltrs of ASM, so I topped up with Methanol and used that.
I can only assume this mix was stronger than your estimate if 80 litres has gelled on supposedly 1.6 litres ASM, I have only ever had gel when I have either overdosed or used wet oil. Mine have been on NAoH though
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An after thought, has your methanol ASM mix been shaken well before use ? maybe it starts to split giving you an stronger dose somehow. Something weird is going on here for you to be having these troubles.
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Third batch with ASM today and yet another batch of gele.
For the Dr pepper and the main batch, I used the ASM/Methanol mix left over from the previous batch. I estimated/calculated that this still contained around 1.5/6 ltrs of ASM, so I topped up with Methanol and used that.
I can only assume this mix was stronger than your estimate if 80 litres has gelled on supposedly 1.6 litres ASM, I have only ever had gel when I have either overdosed or used wet oil. Mine have been on NAoH though
Nope, exactly the same mix used for the Dr Pepper as the main batch.
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An after thought, has your methanol ASM mix been shaken well before use ? maybe it starts to split giving you an stronger dose somehow. Something weird is going on here for you to be having these troubles.
Nope, I've got mixing paddles in the Methoxide drum and the whole lot was mixed well before introducing to the processor.
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What was the 90/10 result on the Dr Pepper and also on your batch ?
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3/27 on the Dr Pepper gave 0.6ml drop out.
Never got as far as testing the main batch ... it went directly from oil to gel after adding about half the catalyst!
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Julian, by now you must be almost out of usable fuel,
do you have enough NaOH to do a batch (as ASM is clearly not working for you right now),
if you haven't I have some you can have mate.
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Julian, by now you must be almost out of usable fuel,
do you have enough NaOH to do a batch (as ASM is clearly not working for you right now),
if you haven't I have some you can have mate.
Yup, just got what's in the Disco tank ... eeek!
Thanks ever so much for the offer, but I have loads of NaOH, typically and stupidly, I ordered 25 Kg just before buying the ASM! It's oil I've now got a problem with. I've exhausted my every day supply, but I do have a small reserve I'll have to dip into.
Now, ask me if I'm short of soap!
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[/quote]
Now, ask me if I'm short of soap!
[/quote]
Julian... r u short of soap?
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Have you checked the methanol?
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Have you checked the methanol?
It's on the list of things to check, but I've no reason to suspect it ... newish drum from known supplier, well sealed, stored in warm dry garage, and has not given any problems in the past.
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Ok, checked my Methanol (gave me the opportunity of some photos for the wiki page I started many months ago!)
Methanol SG is 0.805 @ 10.2°C.
My chart only goes down to 11°C, but that gives 98%. At a lower temperature the purity would be higher so at a guess it must be around 98-99%.
(http://www.palmergroup.co.uk/Bio/Methanol SG1.JPG)
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I suspect that if you methanol was bad, the Dr Pepper sample would have behaved in the same way as the full batch.
Something has got to be happening in the processor that shouldn't be. Is the circulation OK (not a partially blocked pump or similar).
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No blockages. I've got a pressure gauge on the pump discharges (where they are common) and any blockages down stream show up on the gauge. And besides I'm overly cautious of what I put in the processor. The oil is either visibly clear or is filtered through landscaping fabric ... not sure of the micron size but it's quite fine.
The Dr Pepper was only a small sample ... ½ a jam jar, so that could be a reason in it's self, but after some thought the major differences between the Dr Pepper and the batch is copper and temperature. Dr pepper saw no copper, the batch saw lots. The batch was processed at around 60°C and the Dr Pepper was probably down to around 30 - 40°C by the time I tested it.
Anyone else using ASM with a copper processor and pipe work?
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Afraid not, mine is stainless steel with iron pipework and fittings. I would not have thought that copper would have that much effect but I guess anything is possible. Maybe try a doctor pepper with a piece of copper in the jar?
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That was exactly my intention. Got ideas for a series of Dr Peppers which I'll post for comments shortly.
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Julian
you mention copper and asm.I noticed something very strange with the barrel pump i made from copper the asm turned it jet black.Could this be some sort of reaction.
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If I was anything of a chemist I'd stand a fighting chance of answering that and solving the problem I have!
As far as I know when copper oxidises it goes that nice verdigris colour, and that I assume is a reaction with Oxygen.
I guess it's quite possible some alternative reaction happens with ASM. Me thinks an experiment of copper in a high concentration of ASM is called for. I'll pickle and wash the copper first to make sure it's clean.
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If I was anything of a chemist I'd stand a fighting chance of answering that and solving the problem I have!
As far as I know when copper oxidises it goes that nice verdigris colour, and that I assume is a reaction with Oxygen.
I guess it's quite possible some alternative reaction happens with ASM. Me thinks an experiment of copper in a high concentration of ASM is called for. I'll pickle and wash the copper first to make sure it's clean.
Surely it is not the effect of ASM on copper you are looking for but the effect of copper on your reaction using ASM.
ASM at the end of the day is the same as Sodium hydroxide in methanol but without the water. Perhaps if you email Graham Laming he may know.
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Just read this
"Conventional sodium methylate manufacturing processes typically employ mercury-sodium amalgam in the electrolysis process, which could potentially contaminate suppliers’ grades with trace quantities of mercury. In contrast, the unique manufacturing process for DuPont™ Sodium Methylate in the U.S. incorporates innovative technology that virtually eliminates traces of mercury and enhances product purity"
Could our ASM have traces of Mercury that maybe gives rise to problems?
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If I was anything of a chemist I'd stand a fighting chance of answering that and solving the problem I have!
As far as I know when copper oxidises it goes that nice verdigris colour, and that I assume is a reaction with Oxygen.
I guess it's quite possible some alternative reaction happens with ASM. Me thinks an experiment of copper in a high concentration of ASM is called for. I'll pickle and wash the copper first to make sure it's clean.
Surely it is not the effect of ASM on copper you are looking for but the effect of copper on your reaction using ASM.
ASM at the end of the day is the same as Sodium hydroxide in methanol but without the water. Perhaps if you email Graham Laming he may know.
Good point, the Dr Pepper with added copper should highlight any problems, but as ASM is the major change to test it directly with copper can't do any harm, especially in the light of what William says above.
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Looks like I might have some bio at last!
I filled the process with water, heated and circulated in an attempt to remove any residual soap. Rinsed out the Methoxide mixer with fresh Methanol. Dried 80 ltrs. of really good oil to over 100°C and processed using a two stage titrated process which gave a 3/27 with colour but no dropout after half an hour of the second stage. Recovered just over 5 ltrs of Methanol and the Glycerin is settling as I type. I'll drain the lower pipe work later and settle further over night ready for an acid wash tomorrow.
So, Dr Peppers I intend to do are as follows ...
1) The oil I used today with ASM from drum 1.
2) The oil used in the previous failed batches with NaOH, titrated.
3) The oil used in the previous failed batches with ASM from drum 1 and several pieces of pickled Copper
4) The oil I used today with ASM from drum 2( (subject to friends daughter drinking enough pop to get me another test bottle!)
Can anyone think of any other meaningful test that can be carried out?
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Looks like I might have some bio at last!
Dried 80 ltrs. of really good oil to over 100°C and processed using a two stage titrated process which gave a 3/27 with colour but no dropout after half an hour of the second stage.
What were the numbers Julian.
1, Ml of ASM stage 1
2, Ml of ASM stage 2
3, Methanol amount for each stage.
And was this fresh Meth and fresh ASM ?
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It was my usual titrated method as stated ... and I should have said using NaOH, sorry!
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Can anyone think of any other meaningful test that can be carried out?
Try a DP with half strength ASM from drum 1
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It was my usual titrated method as stated ... and I should have said using NaOH, sorry!
At this point I'd normally of called you a quitter, but with your recent results (and fuel situation) this is a very understandable move.
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It was my usual titrated method as stated ... and I should have said using NaOH, sorry!
At this point I'd normally of called you a quitter, but with your recent results (and fuel situation) this is a very understandable move.
Possible good news on the oil front, Got a call from a place I dropped a card at about a year ago, picking up tomorrow. Also got a missed call on my mobile, the number Googles as a local chip shop ... I'll call them tomorrow.
On the bad news front the Golf has started playing up, so I'll be doing some subzero mechanics tomorrow!
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Can anyone think of any other meaningful test that can be carried out?
Try a DP with half strength ASM from drum 1
Thanks Nige,
Restricted for pop bottles at the moment, but if the full strength test goes breasts up, that will be the next one to try.
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To follow on this saga ...
Went to collect the oil from the greasy spoon, having been told it was all dry and liquid ... yeah, right.
About 10, 20 ltr drums, all with the tops missing some overflowing with thick, yellow, frozen fat.
I had higher hopes for the lidded 100 ltr barrel, but no, exactly the same in there. Now got a dilemma as to process in this weather or not.
Anyhow, spent quite a while today carefully doing Dr Pepper tests. First one was with 500ml of really good oil and a base of 3.5 ASM from drum 1 ...
(http://www.biopowered.co.uk/w/images/0/0a/ASM_Dr_Pepper_-_Special_reserve_oil.JPG)
"Special reserve oil"
(http://www.biopowered.co.uk/w/images/b/b7/Adittion_of_half_catalist.JPG)
Half the ASM/Methanol added and shaken lightly ... interesting to see the separation despite the shake.
(http://www.biopowered.co.uk/w/images/a/ae/ASM_Dr_Pepper_vigorous_shaking.JPG)
After vigorous shaking.
(http://www.biopowered.co.uk/w/images/8/81/ASM_DR_Pepper_-_completed_reaction.JPG)
Completed reaction
So, the DR Pepper worked OK. I didn't do a 3/27 test as I only wanted to check I wasn't making soap!
Next test was poor quality oil, very similar or the same as the first batch which went wrong ... that too gave a non soapy, good result.
So thinking now is it's got to be my process.
I'm interested in the light brown, almost opaque emulsion looking mixture after the vigorous shake. I have noticed this, along with a soapy texture, on full size batches if you take samples during or immediately after adding the metoxide. As with the Dr Pepper above, this clears if you carry on adding catalyst and continue to process.
Anyone else noticed this before?
With the above in mind I decided to do a Dr Pepper on the last batch to go wrong. This was still liquid in cubies outside. As I'd added about half the catalyst, I did a Dr Pepper using the 50% base ASM and 50% Methanol (although it was Methanol rich from my attempts to recover it). This test too produced a full reaction with no noticeable soap.
So I'll be having a go at reprocessing the last batch to see if I can get it to complete.
I'll stick further thoughts in a new post, this one's getting rather long!
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Hi Julian
The pic after the vigorously shacking is normal this is a emulsion we have to create prior to any conversion taking place.
Years of sticking my head inside the tank to see what was going on has taught me this and all the other phases it goes through
Paul
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To follow on this saga ...
Went to collect the oil from the greasy spoon, having been told it was all dry and liquid ... yeah, right.
About 10, 20 ltr drums, all with the tops missing some overflowing with thick, yellow, frozen fat.
I had higher hopes for the lidded 100 ltr barrel, but no, exactly the same in there. Now got a dilemma as to process in this weather or not.
Anyhow, spent quite a while today carefully doing Dr Pepper tests. First one was with 500ml of really good oil and a base of 3.5 ASM from drum 1 ...
(http://www.biopowered.co.uk/w/images/0/0a/ASM_Dr_Pepper_-_Special_reserve_oil.JPG)
"Special reserve oil"
(http://www.biopowered.co.uk/w/images/b/b7/Adittion_of_half_catalist.JPG)
Half the ASM/Methanol added and shaken lightly ... interesting to see the separation despite the shake.
(http://www.biopowered.co.uk/w/images/a/ae/ASM_Dr_Pepper_vigorous_shaking.JPG)
After vigorous shaking.
(http://www.biopowered.co.uk/w/images/8/81/ASM_DR_Pepper_-_completed_reaction.JPG)
Completed reaction
So, the DR Pepper worked OK. I didn't do a 3/27 test as I only wanted to check I wasn't making soap!
Next test was poor quality oil, very similar or the same as the first batch which went wrong ... that too gave a non soapy, good result.
So thinking now is it's got to be my process.
I'm interested in the light brown, almost opaque emulsion looking mixture after the vigorous shake. I have noticed this, along with a soapy texture, on full size batches if you take samples during or immediately after adding the metoxide. As with the Dr Pepper above, this clears if you carry on adding catalyst and continue to process.
Anyone else noticed this before?
With the above in mind I decided to do a Dr Pepper on the last batch to go wrong. This was still liquid in cubies outside. As I'd added about half the catalyst, I did a Dr Pepper using the 50% base ASM and 50% Methanol (although it was Methanol rich from my attempts to recover it). This test too produced a full reaction with no noticeable soap.
So I'll be having a go at reprocessing the last batch to see if I can get it to complete.
I'll stick further thoughts in a new post, this one's getting rather long!
You don't say when you added the second half of the ASM and methanol ? I do think a 90/10 at the halfway and final stage would have been informative.
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Hi Julian
The pic after the vigorously shacking is normal this is a emulsion we have to create prior to any conversion taking place.
Years of sticking my head inside the tank to see what was going on has taught me this and all the other phases it goes through
Paul
So you recon this happens with every reaction then?
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You don't say when you added the second half of the ASM and methanol ? I do think a 90/10 at the halfway and final stage would have been informative.
Steve, I was only concerned that I didn't make soap ... which I (think) I've proved. I'm not really concerned what the conversion was, but if you think it will achieve anything I can still do a 3/27.
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It really does look like your issue is with your processor somewhere as opposed to the chemicals or feedstock.
I seem to remember Mark having similar problems and making jelly each batch. I can't remember what he traced it to in the end.
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Hi Julian
The pic after the vigorously shacking is normal this is a emulsion we have to create prior to any conversion taking place.
Years of sticking my head inside the tank to see what was going on has taught me this and all the other phases it goes through
Paul
So you recon this happens with every reaction then?
Yes that's right
The meth and oil dont really mix well so the first phase is to create a emulsion between the two products , as the reaction starts to take place then it speeds up due to the meth being carried into the oil by the bio.
This is one reason why the acertone seems to work as it mixes the meth into the oil much quicker.
Paul
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I guess that phase of the reaction is something that's usually never seen ... interesting.
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It really does look like your issue is with your processor somewhere as opposed to the chemicals or feedstock.
I seem to remember Mark having similar problems and making jelly each batch. I can't remember what he traced it to in the end.
Mine was feed stock related, very wet (more than I thought) gloupy stuff, mainly palm oil and beef dripping.
I just didn't dry it properly.
My setup hasn't changed.
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The last batch to go breasts up is now undergoing washing and looks OK.
I think the problem with the two penultimate batches was probably water due to bubbling using high humidity ambient air. I still haven't recovered anything from the second rogue batch but once I get my heater to make a tosser tube I'll give it a go.
I now don't think there was a problem with the last batch, I suspect it was me getting neurotic!. I was sampling constantly while the ASM was being introduced and I think I panicked upon seeing the emulsion type mix, evident from the Dr Pepper photos above. It had the colour of a batch turning to soap and was defiantly growing soapy stalactites from the sample point, but returning the whole lot to the processor and adding the balance of the ASM produced bio!
With the batch that went horribly wrong, I dried the oil using ambient air and used about 25% reclaimed Methanol which was distilled by the same method. The last batch that worked, although better quality oil, used virgin Methanol and the oil was dried using only the venturi and condenser.
Looking forward to the next, trouble free batch in the next couple of weeks!
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Cool sounds like you have it sussed know Julian
I have never had problems caused by ASM but I did make up a new titration solution with each batch so that could have reflected the strength at any one place in the Ibc.
Let hope you get on well from now
Paul
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Hopefully your problems are now over Julian.
Just need to get to the bottom of Keiths issues now.
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Hope so Nige, I'll find out with the next batch.
Paul, you say ... "titration solution WITH each batch" that could read that you were using ASM for the titration ... was that the case?
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Yes I would use ASM for the titration
5ml ASM -1 L water
I'd better check when I get in just to make sure that's right
Paul
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Yes I would use ASM for the titration
5ml ASM -1 L water
I'd better check when I get in just to make sure that's right
Paul
That must surely be more accurate that using a 0.1% solution NaOH and extrapolating.