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

[Julian]

It was my usual titrated method as stated ... and I should have said using NaOH, sorry!

[nigelb]

Can anyone think of any other meaningful test that can be carried out?

Try a DP with half strength ASM from drum 1

[Head Womble]

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.

[Julian]

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!

[Julian]

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.

[Julian]

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 ...



"Special reserve oil"





Half the ASM/Methanol added and shaken lightly ... interesting to see the separation despite the shake.






After vigorous shaking.





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!

[Carrington]

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

[1958steveflying]

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 ...



"Special reserve oil"





Half the ASM/Methanol added and shaken lightly ... interesting to see the separation despite the shake.






After vigorous shaking.





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.

[Julian]

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?

[Julian]

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.

[julesandtash]

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.

[Carrington]

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

[Julian]

I guess that phase of the reaction is something that's usually never seen ... interesting.

[Head Womble]

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.

[Julian]

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!