Re: [biofuel] Re: Fw: cloudiness (Paul Gobert)

2002-04-19 Thread Keith Addison

Hi Paul, Christian

Christian, my apologies - I know you addressed the question to me, 
but I'm a bit sporadic these days, otherwise occupied, and didn't 
manage it. I was glad Paul picked it up - I think I said previously I 
hoped someone else would chip in rather than your getting advice only 
from me.

Paul, your black oil is interesting, I had some stuff like that, yuk 
- 9.6 ml titration. I wanted to ask the restaurant customers how they 
liked the food but they were all dead. (Joke.) (I think.)

One thing you might try is to warm it a bit and then pour at least an 
equal quantity of boiling water onto it, shake it up, let it settle 
out, the water should take some of the FFAs with it. Somebody 
reported success with this, but I haven't managed to try it yet.

Ken's method works well:
http://groups.yahoo.com/group/biofuel/message/10378

Another point, as you surmised, is the conc aqueous NaOH solution. 
It's certainly a convenient way of mixing it, though there are others 
- see:
http://archive.nnytech.net/index.php?view=12986list=BIOFUEL

It's interesting to know that it can be done, a useful option. But I 
do have reservations about it - adding even that little water won't 
help the process, though it might not hinder it, depending, but then 
again it might. I think it adds a variable, which for tests is 
perhaps to be avoided - you want as few variables as possible. Well, 
that's my view at any rate. Also, for someone who's learning it might 
be an unnecessary complication, especially as there are other ways of 
doing it.

Another reservation is the use of PET bottles. I think it's been 
established that shaking it initially and then leaving it won't 
guarantee maximum completion. You can still be left with unreacted 
TGs, and di- and mono-glycerides. Water and/or too much lye will make 
soap, and if there's anything more than minimal MGs, you'll certainly 
have trouble washing it. Very gentle washing methods like misting 
might get round that, but the MGs will still be left in the final 
product, and you don't want them in your motor.

Todd said some things about this which I think are worth repeating. 
One was that you should be able to subject the processed product to a 
really fierce wash in a blender, without creating a frothy mess. As 
little as 1% mono-glycerides can lead to enormous wash emulsions... 
If no emulsions form under conditions of wild agitation the fuel can 
be counted on as being a completed product. I think that's right.

By the way, this was among the early feedback on Aleks's update of 
the Foolproof method: ... Just started the wash - and it looks 
stellar. No soap at all, just water and oil. That's as it should be.

Todd also posted this advice on shaking: I would encourage anyone to 
shake vigorously for 30 seconds every half hour for about two hours 
in a one gallon environment... Anything less than such levels of 
agitation invite incomplete reactions. I'd do the same with a PET 
bottle, or more. Shaking it more and processing it for longer 
certainly can't hurt it, and might help a lot. These are only test 
batches anyway, nobody's going to get into making their fuel supply 
in a PET bottle. Well, nobody in their right mind anyway. So the 
longer time and a little more work shouldn't matter. Incomplete 
reactions are the devil of home-brewing and I reckon it's worth a 
little more bother to make sure.

Regarding Christian's soap problem, it seemed to be rather 
high-quality feedstock he used, low titration. I doubt his titration 
was that inaccurate that he's having a high-FFA problem.

Christian, I think you should just keep going, you'll get better at 
it, more accurate, and your results will improve. You're doing fine, 
you just need some more practice.

Regards

Keith



- Original Message -
From: Christian [EMAIL PROTECTED]
[snip]

  Anyway, if too much lye forms that sticky gel and too little forms a third
  layer of unreacted WVO, then if I only get a layer of glycerine and a
layer
  of WVO, my proportions should be right, right?.
[snip]
Not a definitive guide as to the quality of the BD.
As an example made two batches of BD from some really well used oil.
(More about this oil in a few days when I do more tests, get more
imformation from the distributers.)
The oil titrated at 9.0ml, pretty well used. Tried neutralising some of the
acidity with lime but this oil refused to transesterify after the treatment.
Titration was definitely lower but even using levels of NaOH appropriate for
the titration on the origional oil, the treated oil/ methoxide mix remained
in one phase.
Going back to the origional oil I made two 1L batches. Both used 250ml of
methanol.
Batch A/. 15ml of conc aqueous NaOH added to methanol, Batch B/. 20ml added
to methanol.Shaken in 2L bottle, set aside. In half an hour both batches had
settled nicely.
The origional oil is almost black, BD/glycerine interface difficult to see
in A/., easier to see in B/. (BD in B lighter in colour)


Re: [biofuel] Re: Fw: cloudiness (Paul Gobert)

2002-04-18 Thread Paul Gobert


- Original Message -
From: Christian [EMAIL PROTECTED]
[snip]

 Anyway, if too much lye forms that sticky gel and too little forms a third
 layer of unreacted WVO, then if I only get a layer of glycerine and a
layer
 of WVO, my proportions should be right, right?.
[snip]
Not a definitive guide as to the quality of the BD.
As an example made two batches of BD from some really well used oil.
(More about this oil in a few days when I do more tests, get more
imformation from the distributers.)
The oil titrated at 9.0ml, pretty well used. Tried neutralising some of the
acidity with lime but this oil refused to transesterify after the treatment.
Titration was definitely lower but even using levels of NaOH appropriate for
the titration on the origional oil, the treated oil/ methoxide mix remained
in one phase.
Going back to the origional oil I made two 1L batches. Both used 250ml of
methanol.
Batch A/. 15ml of conc aqueous NaOH added to methanol, Batch B/. 20ml added
to methanol.Shaken in 2L bottle, set aside. In half an hour both batches had
settled nicely.
The origional oil is almost black, BD/glycerine interface difficult to see
in A/., easier to see in B/. (BD in B lighter in colour)

Yield. A/.  810ml BD, 450ml glycerine.
   B/.   710ml BD, 500ml glycerine.

Glycerine from both batches drained off easily at 25 deg C.
Batch A/. glycerine was still liquid when last seen 6 hours later.
Batch B/. glycerine set after four hours, setting seemed to occur from the
top down even though the beaker was sitting on cold tiles.
From past experience expect both SG and viscosity of Batch B/. to be lower
than that from Batch A/.


 And very little whit residue (soap?) is left on top of the glycerine
layer.
 However, the first wash is very dirty (white, milky cloudy almos foamy).
So
 what should I change to get less soap formation?

Use an oil with less FFA.
Neutralise the FFA in the oil you use.
Titrate your oil and use the ammount of NaOH indicated by the titration.
The oil used here titrated to 12.5g NaOH/litre.
Batch A/. used the equivalent of 12.5g and Batch B/. 16.7g
Better to err on the high hide than the low side especially if you are
processing animal fats or the oil you are using has beef tallow residues in
it.
Use 250ml methanol per litre of oil.

 Can I wash indefinitely (say, three or four times) to remove all soap?

By all means. Make sure that your initial washing is not to vigorous though
as it is easy to loose BD through emulsification in the presence of soaps.
Mist washing combined with prolonged settling works well. Usually only the
emulsion layer between the BD and the wash water requires prolonged
settling.

Would be good to see others have an input to this as these observations are
from processing using conc aqueous NaOH to make the methoxide.
Whilst this method works well for me and the GC results have been
favourable, its not a method which has acheived universal acceptance.

Accounts of others experiences in these areas would be appreciated.
More on that Black Oil later.

Regards,  Paul Gobert.



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[biofuel] Re: Fw: cloudiness (Paul Gobert)

2002-04-17 Thread Christian

Dear Paul,

My third wash left almost crystal clear water, and after settling for 2
daysd, the BD is definitely transparent and non-cloudy.

Today I continued with 4 litres of BD (four 1 liter batches). Im still in
the glys-BD settling stage, and the BD looks much more brownish than my
first batch, and still cloudy. Ill give it a day or so settling to see what
happens.

Anyway, if too much lye forms that sticky gel and too little forms a third
layer of unreacted WVO, then if I only get a layer of glycerine and a layer
of WVO, my proportions should be right, right?.

And very little whit residue (soap?) is left on top of the glycerine layer.
However, the first wash is very dirty (white, milky cloudy almos foamy). So
what should I change to get less soap formation?. Supposedly less water? Can
I wash indefinitely (say, three or four times) to remove all soap?

Best wishes (+ thanks in advance),

Christian

- Original Message -
From: Paul Gobert [EMAIL PROTECTED]
To: biofuel@yahoogroups.com
Sent: Sunday, April 14, 2002 5:18 PM
Subject: Re: [biofuel] Fw: cloudiness



 - Original Message -
 From: Christian [EMAIL PROTECTED]
 To: biofuel@yahoogroups.com
 Sent: Monday, April 15, 2002 2:27 AM
  My batch of BD settled the glycerine out nicely, though the BD still
 seemed a bit cloudy. It was translucent, but not crystal clear... Is this
 suspended water?
 
  I now bubble-washed it (not for long... the first few minutes produced
an
 emulsion of BD+water which seemed murky white-ish/yewllow-ish.
 
  Now Im settling it. The first wash water is very white (almost like
 milk).

 Christian, you could have soap problems. Filter a sample of the BD through
a
 filter paper.  It should filter crystal clear and leave a white soapy
 residue on the paper.
 Whatman No. 1 filter papers are rated at 11 micron.
 Processing may have to be adjusted so that not so much soap is formed, or
 use a gentler washing technique such as mist washing.

  QUESTION: If the BD remains non-crystal-clear after some washing 
 settling, should I take it to 105 deg C for some minutes?

 Have done that in past. BD clears up when heated but cloudiness returns
when
 it cools.
 After filtering I trialed heat drying but no water dropped out, I no
longer
 heat dry, filtering is my final step.

 Regards,   Paul Gobert.



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