Author Topic: Dis ASM, he mighty pow'ful magic! (or ... have I witnessed a reverse reaction) (Read 21073 times)

Julian · « **Reply #15 on:** January 10, 2013, 07:00:27 PM »

Quote from: nigelb on January 10, 2013, 06:42:17 PM

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.

julesandtash · « **Reply #16 on:** January 10, 2013, 07:11:01 PM »

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.

Julian · « **Reply #17 on:** January 10, 2013, 07:18:40 PM »

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?

Oilybloke · « **Reply #18 on:** January 10, 2013, 07:21:06 PM »

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....

Julian · « **Reply #19 on:** January 10, 2013, 08:04:32 PM »

So am I the only idiot trying to use ASM with titration?

1958steveflying · « **Reply #20 on:** January 10, 2013, 08:11:39 PM »

Quote from: Julian on January 10, 2013, 08:04:32 PM

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.

Julian · « **Reply #21 on:** January 13, 2013, 04:29:57 PM »

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 ...

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.

Dr Pepper test, same oil, same catalyst. (sorry, photo a bit dark!)

1958steveflying · « **Reply #22 on:** January 13, 2013, 04:42:48 PM »

Quote from: Julian on January 13, 2013, 04:29:57 PM

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

1958steveflying · « **Reply #23 on:** January 13, 2013, 04:46:04 PM »

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.

Julian · « **Reply #24 on:** January 13, 2013, 04:58:03 PM »

Quote from: 1958steveflying on January 13, 2013, 04:42:48 PM

Quote from: Julian on January 13, 2013, 04:29:57 PM
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.

Julian · « **Reply #25 on:** January 13, 2013, 04:59:33 PM »

Quote from: 1958steveflying on January 13, 2013, 04:46:04 PM

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.

1958steveflying · « **Reply #26 on:** January 13, 2013, 05:30:14 PM »

What was the 90/10 result on the Dr Pepper and also on your batch ?

Julian · « **Reply #27 on:** January 13, 2013, 06:07:18 PM »

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!

Head Womble · « **Reply #28 on:** January 13, 2013, 09:47:58 PM »

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.

Julian · « **Reply #29 on:** January 13, 2013, 10:26:05 PM »

Quote from: mark on January 13, 2013, 09:47:58 PM

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