2 stage bother : (

[nigelb]

I know it's a bit late now to be offering advice and you probably wouldn't have took it anyway but if something has gone wrong and it needs a fix don't go into it with your blinkers on. Do a jug sample first to get your "fix" and then scale it up to your batch size. Other wise, as you now have, you end up with a bigger mess.

It's really simple....for some.

[thewormman]

Would some acid in there have made any difference? Would that have split it?

Still trying to learn...

[julianf]

Who knows. 

I think i may feed the remainder of the batch in with fresh wvo on the glyc wash stage.  As mentioned, ive got full conversion now, but the part that was demethed turned to jelly.


The feedstock of this lot was collected two summers ago, and had more meat in it than would fit in a tesco carrier bag - i really want to get my titration kit back (or make another) as i think it would be worth using on batches like this, to adjust the first stage of the 2-stage.

This batch has all the symptoms of a wet batch, however, i spent more time prep'ing it than normal (both with long cycle heat and settle, and with glyc wash) so im really not convinced it was wet.  I suspect just bad chemical adjustment, probably underdosing on catalyst on the first stage, and then overdosing on meth thereafter.

My usual method is to dose with 15% of the whole batch methanol, and then catalyst to a supposed titration of 2 [koh] (again for the whole batch), and then finish up with 20%+base for the remaining on s2 (which is generally under 10%) - this probably wasnt the time to change the method!


In all the time ive been brewing ive had a total of two jelly batches (this being one of them) and one failed water washing attempt, so, hey, some you win, some you loose (just need to make sure you win most of them!)

[nigelb]

Whatever is wrong with this batch Julian you made a big mistake by not doing a jug sample to find a fix.

You claim a 100% conversion yet there is something fundamentally wrong with the way you conducted the 27/3. ie you have no glyc drop out so your testing that also..
Is having no glyc dropping out constistant with a "jelly" batch? I ask becuase I've never had this issue. Not to say that I won't at some point in the future.

You have an ideal opportunity to really find out what's going on here because you have half the batch to play with.

How much methanol did you recover before it went tits up?

Your brew shed must have been on the point of blowing up with all of that hot, methanol rich bio all over the floor.

[nigelb]

Would some acid in there have made any difference? Would that have split it?

Still trying to learn...

Different things work for different problems. The key is doing some samples in a jug to find out what does work and what doesn't. I had a slight emulsion yesterday after adding the water wash at the end of process. When I tried droping the glyc before pumping into the wash tank i could see there was something not quite right. I mixed it all up again and put some in a jug. I added a bit of stage one glyc to it and mixed it with a thermometer. It returned back to what I would normally expect. So I added 8lts of glyc into the mix and hey ho my problem solved. Easy peasy squeezy lemons

[Head Womble]

When I produced my jelly batches the gly did not drop, but I only got to the first stage when it thickened up.

One of these batches is now sitting in Julians garden, so he'll be able to give more info on how he saves it.

[julianf]

So far, i have tried -

1)Heating in a pan, to make certain there is no methanol remaining. 
Result - cooled to the same thickness, or, possibly, even thicker

2)Warming, and then mixing,50:50, with nice, road-reddy, bio.
Result - 2x as much jelly.


The result that i was wanting with this second test was that, if the soaps were diluted enough that jelly did not form, then they would have a chance to settle out.  And then, if need be, the top (settled) layer could then be used to 'cut' more jelly.

I still think there is hope in this plan.  Either by cutting with a higher percentage, or, i also thought -

Would the soaps settle from jelly if the batch was kept molten for long enough?  Or would the convection currents stop the soaps settling and / or precipitating out?

[therecklessengineer]

1)Heating in a pan, to make certain there is no methanol remaining. 

How hot did you get it? Did any bubbles form? Smell?

I'm trying to correlate against my "heat it until it sorts itself out" approach!

[julianf]

Im sure i wrote it somewhere.... (but evidently not on this thread)

I put it in a pan on the stove.  Heated it, using the IR thermometer to keep an eye on what was going on.

At about 55 ish, i got a few bubbles forming on the surface, but, really, not that many.  They dissipated fairly quickly, and i took the mix up to about 95c, and then stopped.

I think that there was a very small amount of meth remaining, however, not that much, and getting rid of it (unfortunately) made little difference - if anything the mix may have been slightly thicker since.

[Jonzeyboy43]

I thought 27/3 worked regardless of glyc as it is miscible with methanol

[julianf]

Right, an update -

The 100ml of jelly that i 'cut' with 100ml of good bio resulted in 200ml of jelly...

...but i still had hopes for it!

I put it back in a pan, water bath style, and heated it up again, and let it cool slowly (as the water retained the heat with it)

Result -

about 50ml of white soapy jelly / haze in the bottom, and 150ml of good bio on top.  So, taking into account that id added 100ml of good bio, thats 50% recovery.

I then did the same again, and, sure enough, less layer at the bottom.

Ive did it one more time today, and i now have about 20ml in the bottom of the beaker.  So that's 200ml, of which 100ml is the good that i added, and 80ml is the recovered.

Considering i did not take any glyc out of this batch at all, id be happy with 80% product (its certainly better than nothing!)

The 20ml now looks more like glyc than the soapy haze too.  Ie its dark in colour.



I do not know the consistency of any of this, as im not shaking the beaker up at all.  But the top is liquid, and, unless i have perfectly clear jelly lower down, id say its liquid to the glyc layer.

I will tip it out tomorrow to be sure.



From this test, im starting to think that, possibly, jelly batches can be cured by keeping the mix above the jelly melting point, and waiting for the soaps to settle whilst its hot.  I cant do this in my processor, as the heater is inline, so i think im going to try chucking a radiator in a clip-top, and, hopefully, recovering the rest of the batch like that.

[Julian]

Julian, I've forgotten the start of this threadand being a lazy SOB I'll ask to save me reading it all ... At what stage in the production process did the soap/jelly form?

[julesandtash]

Sounds like a good time to get the water heating coil installed in your processor - then you can heat up the jelly with no circulation needed (except the water through the coil of course)

[julianf]

Julian, I've forgotten the start of this threadand being a lazy SOB I'll ask to save me reading it all ... At what stage in the production process did the soap/jelly form?

Demeth.

But the batch was having issues prior - glyc would not drop.  Then on demeth, it thickened up, and started splattering out the suction port of the venturi, as my inline heater cavitated due to lack of cooling flow.

[Julian]

Julian, I've forgotten the start of this threadand being a lazy SOB I'll ask to save me reading it all ... At what stage in the production process did the soap/jelly form?

Demeth.

But the batch was having issues prior - glyc would not drop.  Then on demeth, it thickened up, and started splattering out the suction port of the venturi, as my inline heater cavitated due to lack of cooling flow.

OK, that's a little different to the two batches I made and the one Womble has dumped in my back garden.  Those went to jelly as soon as the meth/ASM was added.  The fix for those appears to be a good mix with glycerine while heating to about 65°C,  settle, drain glycerine and then process as normal, recon I got about 90% yield from the two batches I've done so far, yet to try Marks stuff in the processor.