Author Topic: Two stage process with no titration  (Read 11303 times)

Offline John Galt

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Two stage process with no titration
« on: July 14, 2014, 07:08:50 AM »
At
http://www.biopowered.co.uk/wiki/Two_stage_process_with_no_titration

The formula states that 2nd stage is
remaining 20% of the methanol" with "unprocessed oil volume x base" catalyst.

however when one runs the example for 100 liters through the calculator at
http://www.biopowered.co.uk/forum/tools/notitration.php
with 10% drop-out,  the calculator does not show 4 liters for the amount of 2nd stage methanol required, [ie."remaining 20% of the methanol"]  instead it shows 2 liters, as if one was calculating the amount of methanol at 20% for the 10 liters of unreacted VO.

Which is correct?  The formula posted, or the calculator?


Offline julianf

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Re: Two stage process with no titration
« Reply #1 on: July 14, 2014, 07:40:00 AM »
The methanol should be added for the remaining, unconverted, only.

I would also suggest that 20% (of the remaining) is excessive, as there will be residual methanol in the solution from stage 1.

Personally, i use 10% (of the unconverted), however, im sure others do differently.
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Offline Tony

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Re: Two stage process with no titration
« Reply #2 on: July 14, 2014, 10:15:13 AM »
Ah - yes, this is probably a hangover from the older days of experimenting with two stage processing.

Essentially, both should work.  But you may save some Methanol by using 20% of the unreacted volume, rather than just dumping in the remaining Meth/Methoxide mix that you have.

Excess Methanol is never a problem aside from the extra cost of Methanol, and having to recover more at the end if you're into reclaiming the excess Meth for the next batch.  We will amend the wiki page - thank you for your input :)

Offline julianf

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Re: Two stage process with no titration
« Reply #3 on: July 14, 2014, 10:26:09 AM »
Tony,

I think excess meth can be an issue.  I made a pigs ear of a batch ages back, when i kept adding catalyst + 20% meth (of the unconverted) on a batch that would not drop the glycerol.

In hindsight, i now realise that my 90/10s were (probably) being thrown off by the glyc still in solution, and i just kept on adding meth : /

What i should have done is add the caustic in a small amount of meth, and it would probably have split, but i wasnt smart enough for that (or it was late, i was covered in oil, frustrated, and all the rest - as usually happens when it goes wrong!)


Anyhow, im sure that, at the end of the mess, it was the excess methanol messing things up. 
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Offline John Galt

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Re: Two stage process with no titration
« Reply #4 on: July 15, 2014, 09:54:58 AM »
"this is probably a hangover from the older days of experimenting with two stage processing."

Which is "a hangover"?  Is the calculation page valid?

Where is the current information on two stage 'no titration' processing?

Offline Tony

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Re: Two stage process with no titration
« Reply #5 on: July 15, 2014, 10:04:22 AM »
"this is probably a hangover from the older days of experimenting with two stage processing."

Which is "a hangover"?  Is the calculation page valid?

Where is the current information on two stage 'no titration' processing?

Hi John, yes it is.

Initially when we were experimenting with titrated two stage we would mix up the methoxide as per normal for a single step batch, but split it into two steps, the first using 80% of the methoxide, draining the glycerol, then putting the remaining 20% of the methoxide back in.

But the titrationless two stage requires measuring the unreacted volume after stage 1.

Because the process was evolved, I think the wiki page still had a guideline the followed the titrated two-stage process (this was the hangover from the titrated process).  This has been updated now to reflect that this was not correct, both the wiki page and the calculator should now tally.

In summary, for stage 2:

  • measure the dropout and calculate remaining unprocessed oil, this is used to calculate the methoxide as follows
  • "unprocessed oil volume x 20%" methanol
  • "unprocessed oil volume x base" catalyst

Offline John Galt

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Re: Two stage process with no titration
« Reply #6 on: July 16, 2014, 05:33:29 AM »
Is anyone using this 'no titration' method with consistent success?

While updating the wiki page it might be a good idea to modify this statement to be more understandable

"what you are doing is a softly softly approach"

Why  "softly softly"  ??
« Last Edit: July 16, 2014, 05:39:54 AM by John Galt »

Offline julianf

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Re: Two stage process with no titration
« Reply #7 on: July 16, 2014, 07:58:39 AM »
Is anyone using this 'no titration' method with consistent success?

Consistent, yes.  Constant, no.

I very much doubt anyone has constant success with any method that they do not modify, on the fly, with their experience.

At the start, your experience will be lacking, so luck will be required also (and asking for help if needed).

"softly softly" -

You do something softly.  And then you do a bit more in a soft way.

Ie you add a smaller amount of base than otherwise.  And then you add a small amount again.
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Offline Jamesrl

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Re: Two stage process with no titration
« Reply #8 on: July 16, 2014, 12:59:26 PM »
If you don't want to use the softly softly approach you could always move on to the slightly more advanced method, the slowly slowly catchy monkey reaction, I've never had a bad batch using it.

Offline willbuild

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Re: Two stage process with no titration
« Reply #9 on: July 16, 2014, 02:47:14 PM »
some batches need 12grs or less base (Kohl), some need 18, 20 grs. I do a Dr pepper test using a base of 12 to give me a guide.
I think that some of the more experienced on here can tell just by looking at the wvo.
 Or maybe theres a taste test :o
« Last Edit: July 16, 2014, 02:51:09 PM by willbuild »

Offline Tony

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Re: Two stage process with no titration
« Reply #10 on: July 16, 2014, 03:34:22 PM »
The very best brewers rub themselves in the oil then see how far they slide on a succession of tarps to work out what reaction method to apply.

Offline willbuild

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Re: Two stage process with no titration
« Reply #11 on: July 16, 2014, 04:58:03 PM »
Is that like a tit test, average of three trails? :D

Offline Jamesrl

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Re: Two stage process with no titration
« Reply #12 on: July 16, 2014, 05:30:59 PM »
I work with me own method, if it looks like it, smells like it and tastes like it it is without doubt WVO so I use it, job done.

Offline K.H

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Re: Two stage process with no titration
« Reply #13 on: July 16, 2014, 06:46:27 PM »
Yes, consistent success using this method and ASM

Offline Jamesrl

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Re: Two stage process with no titration
« Reply #14 on: July 16, 2014, 07:48:46 PM »
Yes, consistent success using this method and ASM

An' I don't not neva get bad batches wiv ASM, been using it for years now, y'can't wack it for supa bio.