Hi Jim,
You wrote:
"I was intially trying different KOH concentrations because I was not
passing the wash test; I assumed that this was due to better-than-expected
KOH quality"
and
"As I reduced KOH concentration, my wash test results worsened and the
methanol test indicated incomplete reactions so I reversed course and began
increasing KOH concentration.- I found that I can pass the methanol test
with higher KOH concentration (5.9 g/L & 6.1 g/L)."
5.9g KOH/L and 6.1g HOH/L -----> pass the methanol Quality Test.
Success with 5.9 g KOH/L indicates that the KOH you are using is about 83%
pure ....
that is, if this veg oil has no Free Fatty Acids.
Given a successful quality test, the emulsion you observe in the wash test
is likely due to the presence of soap. 18 hours of settling time ought to be
sufficient especially given a complete reaction. I suspect that there was
glycerin contamination in the wash.
>At this point, I think I have isolated the source of my wash problems to:
>(1) incomplete separation of glycerin (I just purchased a separatory funnel
>that will >accomodate my test batches to eliminate this problem... I didn't
>have the sep funnel for >those batches)" ..... the 5.9 & 6.1 g KOH/L
>batches that passed QT but failed wash.
Be careful to exclude glycerin from the wash, even if it means draining
a bit of BD with the glycerin. The last time I had a problem w. soap was
whenI accidently drained some glycerin into the wash tank.
>I will mix another batch using 5.9 g/L for 20 - 30 minutes; if I pass the
>methanol test, >can I assume that I'm getting a complete reaction? -
Yes
That is, by the way, the hard part. Focus on achieving a complete reaction
.... passing the methanol test. 5.9g of your KOH/L of this veg oil seems
to be correct.
You might try titrating the oil you are using. a recent post suggested
titrating all veg oil, even unused. I recently titrated a store brand veg
oil and it required 0.3g 90%KOH to neutralize the FFAs present. Another
unused oil titrated 0.7g KOH/L. You will have to become familiar with
titration for the next step.
Good luck. It sounds like you are on the verge of success. You will be
thankful later for the effort you put in now.
Tom
----- Original Message -----
From: "James Pfeiffer" <[EMAIL PROTECTED]>
To: <sustainablelorgbiofuel@sustainablelists.org>
Sent: Tuesday, April 29, 2008 8:13 PM
Subject: Re: [Biofuel] biodiesel test batch question
Thanks Tom and Keith for your responses. > > Have you not gotten complete
reactions on 1L test batches run at 130F > (or higher) in a blender for 20 -
30 minutes?> You are using new, unused veg oil?> Tom - I am using new,
unused soybean oil.- I was intially trying different KOH concentrations
because I was not passing the wash test; I assumed that this was due to
better-than-expected KOH quality (I only received a "represenative
Certificate of Analysis" with the product, not a batch assay). I did not do
the methanol test which, in retrospect, was a mistake. As I reduced KOH
concentration, my wash test results worsened and the methanol test indicated
incomplete reactions so I reversed course and began increasing KOH
concentration.- I found that I can pass the methanol test with higher KOH
concentration (5.9 g/L & 6.1 g/L). I have not tried a titration yet because
I am using fresh oil. Both 5.9 and 6.1 g/L appear to be too high because
that concentration yields a complete reaction and when washed separates
reasonably quickly but the wash results in 1/4" to 1/2" of emulsion, some of
which will break after a couple of days leaving behind chunks of soapy crud
- I ran another batch at 5.8 g/L last night taking extra precaution with
measurement and clean glassware; I allowed the glycerine to settle out for
18 hours in a separatory funnel. Unfortunately this batch failed the
methanol test (there is a bubble of undissolved oil about 0.5 cm in diamter)
and subsequently failed the wash test (fairly quick separation into an oil
fraction and what appears to be a homogeneous emulsion fraction. - w.r.t.
<Are you guessing?> - I have not reduced processing time only because I
wanted to take that variable out of the mix; I will mix another batch using
5.9 g/L for 20 - 30 minutes; if I pass the methanol test, can I assume that
I'm getting a complete reaction? - Regarding measurements:
+ I am still using a simple Ohaus triple beam balance accurate to only 0.1g+
I purchased lab-quality glassware for volumetric measurements+ I began
blending methoxide in larger quantities to try to improve weighing accuracy-
At this point, I think I have isolated the source of my wash problems to:
(1) incomplete separation of glycerin (I just purchased a separatory funnel
that will accomodate my test batches to eliminate this problem... I didn't
have the sep funnel for those batches)
(2) too much KOH (in the case of the 6.1 g/L batch)or, (3) water
contamination in my methanol or KOH
Subsequent wash tests often pass after the initial failure, albeit with
reduced yield. Presumably some of the fuel was emulsified and lost. I will
make my next batch using a different methanol supply to see if that improves
results.
> From: [EMAIL PROTECTED]> To:
> sustainablelorgbiofuel@sustainablelists.org> Date: Tue, 29 Apr 2008
> 07:56:31 -0400> Subject: Re: [Biofuel] biodiesel test batch question> >
> Jim,> > As I write this email, I'm running another test batch. the oil was
> heated > > to 148F >before putting it into a cold blender. When I started
> > > processing, the mixture was 122F >and 42 minutes later it is at 145F.
> I'm > > processing 40 minutes instead of the 20 to 30 >minutes recommended
> on > > Journey-to-forever just because I'm trying to ensure a >complete
> reaction.> > Have you not gotten complete reactions on 1L test batches run
> at 130F > (or higher) in a blender for 20 - 30 minutes?> You are using
> new, unused veg oil?> Tom> > ----- Original Message ----- > From: "James
> Pfeiffer" <[EMAIL PROTECTED]>> To:
> <sustainablelorgbiofuel@sustainablelists.org>; >
> <biofuel@sustainablelists.org>> Sent: Tuesday, April 29, 2008 12:26 AM>
> Subject: Re: [Biofuel] biodiesel test batch question> > > >> > Hey Mike.
> I'm a novice too but, for what it's worth, in my first 10 test > > batches
> in a blender I have gotten a pretty substantial temperature > > increase
> during mixing - between 10F and 20F increase depending on how > > long I
> mixed the batch (from 25 to 45 minutes) and whether it was my > > first,
> 2nd or 3rd batch of the evening (basically "preheating" the > > blender).
> In my first couple of batches I tried to insulate the blender > > with a
> towel because I was worried that the mixture would cool during > >
> blending. After I saw such significant temperature gains, I took off the >
> > towel. I believe that the temperature increase is due to friction of the
> > > blades - I don't know if it is an exothermic reaction.> >> > As I
> write this email, I'm running another test batch. the oil was heated > >
> to 148F before putting it into a cold blender. When I started processing,
> > > the mixture was 122F and 42 minutes later it is at 145F. I'm
> processing > > 40 minutes instead of the 20 to 30 minutes recommended on >
> > Journey-to-forever just because I'm trying to ensure a complete
> reaction.> >> > Hope that's useful.> >> > Jim> > > Date: Tue, 29 Apr 2008
> 12:49:05 +0900> To: biofuel@sustainablelists.org> > > > From:
> [EMAIL PROTECTED]> Subject: Re: [Biofuel] biodiesel test > > >
> batch question> > >Methanol shouldn't vaporize until 148.46 deg F > > >
> assuming the atmospheric> >pressure in you area is 760mmHg.> > That's > >
> > the boiling point of methanol. It starts to evaporate at much > lower >
> > > temperatures than that.> > Temperature maintenance is one of the
> reasons > > > we recommend a > mini-processor rather than a blender: "You
> can use a > > > spare blender, > or, better, make a simple Test-batch
> mini-processor."> > > >
> http://journeytoforever.org/biodiesel_processor7.html> > Another reason >
> > > is that processing in a blender doesn't scale up well > to a
> full-sized > > > processor, blenders are too fast.> Scaling up:> > > >
> http://journeytoforever.org/biodiesel_processor.html#scale> > Best> > > >
> > Keith> > > >Best,> >Chris> >> >> -----Original Message-----> >> From: >
> > > [EMAIL PROTECTED]> >> > > >
> [mailto:sustainablelorgbiofuel-bo> > [EMAIL PROTECTED] On
> Behalf> >> Of Steve Moran> >> Sent: Monday, > > April 28, 2008 4:46 PM> >>
> To: > > sustainablelorgbiofuel@sustainablelists.org;> >> > >
> sustainablelorgbiofuel@sustainablelists.org> >> Subject: Re: [Biofuel] > >
> biodiesel test batch question> >>> >> I think (but I'm not sure) that > >
> methanol will evaporate at 140, is that> >> correct? If it is, then > >
> keeping the temp below that would become very> >> important too.> >>> >> >
> > ________________________________> >>> >> From: > >
> [EMAIL PROTECTED] on behalf of> >> > >
> Thomas Kelly> >> Sent: Mon 4/28/2008 6:39 PM> >> To: > >
> sustainablelorgbiofuel@sustainablelists.org> >> Subject: Re: [Biofuel] > >
> biodiesel test batch question> >>> >>> >>> >> Mike,> >> Test batches can >
> > be difficult ...... well worth the effort.> >> Blenders provide
> excellent > > agitation, but it is difficult to> >> maintain> >> the
> proper temp.> >> > > PET bottles allow one to maintain temp better, but
> agitation may> >> be> > > >> inadequate.> >>>> > >> It is important to
> maintain temp even if you must interupt> >> > > >> agitation.> >>
> Suggestion: Achieve the temp of 130F, blend for 5 > > >> minutes, check
> temp> >> If necessary, carefully return the liquid to a> > > >> >>
> container> >> to be heated.> >> Return to blender and repeat 2 (3?) > > >>
> more times> >>> >> I use a hot water bath for heating the mix. Do you > >
> >> have a pot big> >> enough to fit the blender pitcher into? The pot > >
> >> would contain hot> >> (~150F)> >> water. Instead of pouring the hot mix
> > > >> back and forth you could simply> >> place> >> the pitcher from the
> > > >> blender, with top on, into the hot water bath to> >> re-establish
> the > > >> 130F, blot dry and buzz it again.> >>> >> I have returned to
> doing some > > >> test batches. I favor heating the> >> mix in> >> a PET
> bottle that has > > >> a wide mouth with a twist open/close top. Sport> >>
> drink> >> plastic > > >> bottles often have this feature. This allows me
> to limit> >> methanol> > > >> >> evaporation while heating the mix. I
> either twist the top to open > > >> while> >> heatin> > g or I squeeze the
> bottle to decrease volume of air before> >> closing > > and> >> heating.
> The wide mouth and a funnel make it easy to add the > > liquid. I> >>
> heat> >> the mix in a hot water bath.> >>> >> Good Luck,> >> > > Tom> >>>
> >>> >> ----- Original Message -----> >> From: "mike" > >
> <[EMAIL PROTECTED]>> >> To: <biofuel@sustainablelists.org>> >> Sent: > >
> Monday, April 28, 2008 3:57 PM> >> Subject: [Biofuel] biodiesel test batch
> > > question> >>> >>> >> > Hello everyone, my first post> >> >> >> > i
> want to > > apologize if this has been answered, but I have searched> >>
> the> >> > > > archives and relevant sites without finding a clear answer.>
> >> >> >> > > > I've been reading the j2f howto for doing my first test
> batch with> >> > > > unused veg oil and a blender. I see that I'm suppose
> to pre-heat the> >> > > oil> >> > before starting the process to 130 deg
> F, but everything else i > > read> >> > says I need to maintain that
> temperature which isn't possible > > without> >> > moving the oil back to
> another container t> > hat can be heated.... so I> >> > guess basically
> i'm asking, is that temp > > (130) required for the> >> reaction> >> > or
> does it just aid in a faster > > reaction.> >> >> >> > Thanks> >> > Mike>
> >> >> >> >> > > > > > _______________________________________________> >>
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