Curry oil cock up.

[Tony]

If the meth turns out to be OK, how about drying it thoroughly (maybe heat to 120C to make absolutely sure there is no trapped water) before reprocessing?

I'd try burning a bit of this dried batch in a  jam-jar lid to see if any residue is left (beyond soot).

How does a 50:50 water shake look?  Lots of of emulsion?  (I'm not sure what that would tell us beyond known partial conversion - but, you never know, it might come out clear in which case more thinking is required!)

[Glycer-rides]

B0llocks, I've just spent 20 mins updating the thread without being logged in.

Clear pass obtained!
I will type it out again when the will to live has been re-established...

[Tony]

Stop teasing, how did you fix it?

[Glycer-rides]

I had the Dr P methoxide left, so I re-dosed it very heavily, just to establish conversion was possible. It was!

Based on the 18% u/c in the batch, I mixed up 20% meth @ 6 g/l, bearing in mind my unwisely depleted start point.
No dice after 90 mins.
Being late, I mixed up a 'pint plus a handful', ran for 60 mins, drained a sample and sodded off to bed in a mood.
Tonight, the sample looked a good split, drained the glyc and got a normal quantity and a 10/90 clear pass.

I will post up my 'learning points' later...

[Tony]

I mixed up a 'pint plus a handful'

I'm glad it's not just me that does this.

"Just a dash of catalyst, and a splash of methanol to taste"

As used by all the finest television chefs.

[dgs]

The guy that I collect the chemical rich glycerol from has never weighed his catalyst or measured his methanol. When I asked him how he measures his KOH he said X number of scoops, however the mood takes him.

He has never done a dropout test. I once (couple of years ago) took him a 3/27 tube and explained how to do the test, he never bothered.

[Chug]

sounds a bit like mine, just under a 20L drum of meth (inc 25% recovered) and then a tub and a half of NaOH if the oil is good, or a tub and three quarters if its not so good

[Glycer-rides]

I'm usually as accurate as I can be with the vols and masses.
It didn't show results in this case, so the artisan flair was an uncharacteristic moment.

Points:
As Dave has mentioned, I'm thinking I've glyc washed with excessive soaps being carried over.
I'm finding KOH glyc takes much longer to settle vs NaOH glyc, which might have stalled the stages. Not enjoying the K experience so far...
5 g/L KOH doesn't seem enough for my process.
Not having a stable source of wvo makes things harder!

[Glycer-rides]

Update!

Whilst my crystal clear pass 10/90 is still crystal clear some days later, there is some small amount of white drop out which started to appear after 24 hrs.
It comprises tiny, white soapy flakes. Not wvo coloured as would be expected.

I did a 1/9 on someone else's bio (water washed and settled for an age...gives a much nicer 50/50 than mine)  - same white drop out.

Obviously, the only common denominator here is the meth used for the tests. This is quite new, Trinity reclaimed meth.

Ideas??

[Tony]

White fallout could be waxing, but it seems a little unlikely at these temperatures...

[Glycer-rides]

Here's an update, as we like updates...

Well, this bio has been fine in my new 250bhp/540Nm brown trouser CDi.

Just started another batch.The processor was pre-loaded with more of this orange wvo, so I had no feedstock choice.

Same lack of reaction crapness transpires.
 
At this point, all I'll say is that this Trinity reclaimed (that smells of solvent) when mixed with Trinity KOH, turns the colour of bio.
That's not right, IME.

Off to the pumps mid week, then.

[dgs]

The Trinity reclaimed methanol is certainly wierd stuff as far as appearance and smell goes. The last IBC I had also had a colour to it. Having said all that, the reactions are completley normal.

When processing, if the last reaction glycerol isn't given enough time to settle and be removed then any chemicals added from the 10/90 findings will result in a lot of them being absorbed by the glycerol.

Using low temperatures for the first reaction/s and a minimum of methanol seems to slow the glycerol dropping out of the process. If I leave each reaction overnight so most of the glycerol can be removed then the chemical addition from the result of the 10/90 is quite accurate. This is one of the reasons that I use no heating at all for the initial reaction/s at this time of year.

[Glycer-rides]

Thanks Dave.

I started at 60C, minimal method 11% and 6.5 g/l of KOH. Eductor mixed for 2 hours.

With nothing happening, the meth was incrementally increased, ending up at 13.5% with nothing happening.

I then did what I did before. About 250g in a litre or so. An hour of mixing and a good split looked evident before I went to bed.
I hope to find that I've single staged it, when I check the conversion later!

I suppose it's taken 9 g/l thus far. This KOH is not old and has been well stored.
An ode to titration...?

[Glycer-rides]

Not enough meth handy in my 10/90 test supply bottle, so I had to do a syringe 1/9 for indication only with what was left.

Looks to be c. 70% converted.

[Glycer-rides]

Bit of an update for y'all.
The subsequent batch of good wvo went fine, no glyc wash was done.
This weekend's batch was fair wvo and was K glyc washed...and ****, we're back to 3+ stage buggeration.

Despite long settling and done at 60C, my K glyc. just doesn't seem to drop out fully, then when processed I get the knock on effects.

I can't wait to get back to Na...