Roger,
I'm stumped by the third photo. Why so much soap when you used new veg
oil.
I'm surprisd it separated at all.
You are certain the methanol is dry?
Soap forms when there is water contamination.
Soap forms when Free Fatty Acids are present.
Ken P. responded to you on March 31:
"It's ALWAYS a good idea to titrate, even virgin oil. Many oils,
including palm and olive (don't know about peanut) have high FFA levels as
typically sold."
The reason for using new, unused veg oil of our first test batches is
to decrease the number of variables we are dealing with. It is best to avoid
titration until you get the basic process under your belt. It is assumed
that new oil doesn't have to be titrated. This may not be the case.
Suggestions:
1. Pick up a container of "Heet" (brand of gas line antifreeze) Yellow
container, NOT Red. (If it is available to you.) ~ $1.50/300ml. (US).
It is dry methanol.
2. I did my test batches using a name brand corn oil. The people I have
helped in my "neigborhood" have done the same. We had no problems with FFAs.
Maybe you should invest in a bottle of name brand corn oil ..... or is
that what you already did?
As for pH meters: (Ken P):
"pH really only makes sense when referring to a water-based solution.
Sticking pH paper or pH meter into biodiesel gives spurious results
in most cases. I often measure the pH of my wash water as a check
of how much lye and soaps may be left in the biodiesel, but never the
biodiesel (or oil) itself."
Get Phenolphthalein (dissolved in alcohol) for titrations.
We'll deal with the mysterious peanut oil and with you WVO after you
succeed w. the test batches.
I'm now curious about peanut oil. I'll see about getting some and
doing a test batch myself.
Tom
----- Original Message -----
From: "Roger" <[EMAIL PROTECTED]>
To: <sustainablelorgbiofuel@sustainablelists.org>
Sent: Wednesday, April 02, 2008 2:50 PM
Subject: Re: [Biofuel] Test Batches with Peanut Oil
New Results...Better I think.
I tried another batch last night with vegetable oil with 'better' results.
1L Clean, Virgin, Vegetable Oil
200ml Methanol
5.5g of 90% KOH (All with very similar results)
55°C Temp via Hotplate
Agitation: Fast Stirring for 30 minutes via Hotplate
Here are some pictures of what I have so far...
http://tesi.servepics.com/roger/BD-4208-01a.JPG
http://tesi.servepics.com/roger/BD-4208-01b.JPG
http://tesi.servepics.com/roger/BD-4208-01c.JPG
I let it settle for 14 hours. Picture A is of the results.
Picture B is right after shaking 20ml of BD and 20ml of water (both at
room temperature)
Picture C is after an hour of settling. The is the best wash test I've
gotten but it looks like a lot of soap in there.
So my question is... which way do I need to go to make it better? More
KOH? I'm using very accurate measurements. (Digital balance accurate
to 0.001g, Graduated cylinders, etc.) No water contamination that I'm
aware of and taking precautions not to have any. That is the only thing
missing from J2F, pictures with typical results and adjustments
necessary to make improvements. Haven't tried the methanol test yet
(still at work).
Now, when I used peanut oil with the same recipe, I got a cloudy, opaque
water and cloudy whiteish BD after the wash test. Any thoughts on which
way I need to go with that? I presume I'll have to titrate it and make
adjustments from there. I need a pH probe to go with my meter before I
can proceed with the peanut oil or used oil.
Thomas Kelly wrote:
> Roger,
> Now we're getting somewhere.
>
>
>> The original separation looks great - waited at least 12 hours but
>> separates in about 2 hours. Obvious layers with a slightly hazy, pale
>> yellow biodiesel layer and clear, darker by-product layer.
>> Separated by pouring the biodiesel off the top. Looks to be about 1.1L
>> of biodiesel for each batch.
>>
>
> You are getting a clear split. You have made biodiesel. You may well
> have some unreacted mono and di glycerides in with the BD.
> - Have you tried a quality test on the unwashed biodiesel?
> i.e. the Jan W. solubility in methanol test describes at JtF?
>
> - I would be very careful not to include any glycerin mix when you pour
> the
> biodiesel off the top. In fact I would avoid pouring altogether. Draw the
> BD
> off using a pipette or do the following: Get a few .5 L - 1L clear
> plastic
> sports drink bottle (PET bottles) that have twist open/close tops. Some
> water bottles have pull-to-open push-to-close tops. Process as usual,
> allow
> to cool a bit and then pour the mix into one of the bottles. Allow the
> biodiesel-glycerin mix to settle in a closed and inverted bottle. After
> 12 -
> 24 hours drain out the glycerin from the bottom.
>
> If any unreacted glycerides are present, even a small amount of
> glycerin/soap contamination will prolong separation time during the wash
> test.
>
>
>> With each wash test I got cloudy water with a very
>> thin white line between. The biodiesel looks cloudy white.
>> With each wash test I got cloudy water with a very thin white line
>> between.
>>
>
> Do you mean:
> Cloudy water on bottom, with a "very thin white line between" the cloudy
> water on bottom and something darker on top?
> This would be a good thing.
>
> When you say: "The biodiesel looks cloudy white." I'm a bit confused. If
> the biodiesel is white, you wouldn't be able to see the "very thin white
> line between". It would just be white on top of white.
> Is the biodiesel layer (on top) darker than the "thin white line"?
> Again,
> a good thing.
>
>
> >However, it doesn't look quite like what J2F described as good fuel.
>
> Do you mean after doing a wash test?
> It will not yet be good fuel. It will take more than shaking with water
> once
> to get the contaminants out of the BD.
> After 3 or 4 washes, the wash water should be clear and the same pH
> as
> the water that was added. The BD will be cloudy because water will be
> suspended in it. The next step is to dry the BD. Heat it gently. You might
> put your tube of BD in a hot water bath. As the mix heats up water will
> fall
> out and the BD will clear.
>
> I do my wash tests in the same PET bottles described above. Equal
> volumes of water and BD ~150ml of each. Shake vigorously. With top
> closed, invert, and drain after water settles out. Add clean water &
> repeat.
>
> >The last batch of 6.0g separated the quickest, less than a minute - the
> others
>
>> longer up to 15 minutes or so.
>>
>
> It might be that your KOH is not 90% pure
> @ 90% purity you would use 5.45g KOH/L of unused oil
> @ 85% purity you would use 5.76g KOH/L of unused oil
>
> Doing the methanol quality test on the BD before you wash it or after you
> wash and then dry it would tell us more about your success in achieving a
> complete conversion of the veg oil.
>
>
>> And, with the rest of the batch in a jar in the garage, each one has
>> turned
>> to mush. >Looks like the inside of a melon or something.
>>
>
> You're losing me here. Are you referring to the glycerin mix separated
> from
> the BD?
>
> Just another word of caution. When you do succeed at 1L test batches and
> feel comfortable w. the process. scale up gardually. We can talk aboput
> this
> another time.
> Dinner calls.
> Best of Luck to You,
> Tom
>
>
>
> ----- Original Message -----
> From: "Roger" <[EMAIL PROTECTED]>
> To: <sustainablelorgbiofuel@sustainablelists.org>
> Sent: Monday, March 31, 2008 1:41 PM
> Subject: Re: [Biofuel] Test Batches with Peanut Oil
>
>
> Sorry for the excitement and frustration. I've made 4 or 5 1L batches
> with virgin peanut oil with no luck.
>
> 1L Clean, Virgin, Peanut Oil
> 200ml Methanol
> 5.4g, 5.5g, 5.6g, 6.0g of 90% KOH (All with very similar results)
> 55°C Temp via Hotplate
> Agitation: Fast Stirring for 30 minutes via Hotplate
>
> The original separation looks great - waited at least 12 hours but
> separates in about 2 hours. Obvious layers with a slightly hazy, pale
> yellow biodiesel layer and clear, darker by-product layer.
> Separated by pouring the biodiesel off the top. Looks to be about 1.1L
> of biodiesel for each batch.
>
> It's slightly colder in my garage, but not outside temperate. I'd say
> roughly 55°F or so. Each wash test was with 20ml of product and 20ml of
> water in a 50ml plastic tube. The final wash test I performed inside
> with warmer water. With each wash test I got cloudy water with a very
> thin white line between. The biodiesel looks cloudy white. The last
> batch of 6.0g separated the quickest, less than a minute - the others
> longer up to 15 minutes or so. However, it doesn't look quite like what
> J2F described as good fuel. And, with the rest of the batch in a jar in
> the garage, each one has turned to mush. Looks like the inside of a
> melon or something.
>
> My first thought was that peanut oil was different enough from vegetable
> oil that I would need to titrate it and change the KOH amount. However,
> I wasn't having much luck with the pH meter. One time it would be add
> 0.4gm of KOH and the next time 0.01g would be too much. I thought I
> didn't know how to use the meter.
>
> The processor I made (assuming I would be using it by now) has 2) 75
> gallon tanks with individual heaters, controls, pumps, and stirrers. It
> can be used as a 150gal unit or a 2-stage 75gal unit. (I've attached a
> picture.) I can't wait to try it but haven't used it yet for fear of
> making a lot of soap.
>
> Your thoughts are greatly appreciated.
>
>
>
>
> Thomas Kelly wrote:
>
>> Roger,
>> Back up a bit.
>>
>>
>>> Has anyone tried this? It's all I had laying around to start with but I
>>> keep getting a questionable result.
>>>
>>>
>> By "tried this" do you mean peanut oil?
>> If so, I have run batches with peanut oil mixed in.
>>
>>
>>
>>> Since it was new, I tried the same recipe for virgin vegetable oil and
>>> it
>>> didn't really pass >the wash test and as soon as it got cold, it turned
>>> into sludge.
>>>
>>>
>> Got cold??? The wash test is done at room temp 70-ish F
>> (20-ish
>> C)
>>
>>
>>
>>> I made a 2x75Gal machine that I
>>> am dying to use and the used oil is piling up.
>>>
>>>
>> (What's a 2x75Gal machine? .... a 75 Gal processor? 150 Gal processor?)
>> Hold on now cowboy ..... let's not sign up for a marathon run before we
>> up
>> and walking. You don't want to turn gallons of good oil into gallons of
>> goop.
>>
>> You might start by telling us step-by-step what you are doing.
>> Ex 1L fresh, unused vegetable oil
>> 200ml methanol
>> 5.45 g of 90% KOH
>> Method of agitation?
>> Temp?
>> 30 minutes reaction time
>> Do you get a clear split?
>> How long do you let it settle?
>> How do you separate the settled glycerine mix from the biodiesel
>> (separatory funnel?)
>>
>> Describe the results of the wash test, done at room temp, as to time for
>> separation + appearance of layers.
>>
>> While it is important to be able to measure accurately, especially for 1L
>> test batches, I have gotten along fine w/o a pH meter.
>> Best Wishes,
>>
>> Tom
>>
>>
>> ----- Original Message -----
>> From: "Roger" <[EMAIL PROTECTED]>
>> To: <biofuel@sustainablelists.org>
>> Sent: Monday, March 31, 2008 10:13 AM
>> Subject: [Biofuel] Test Batches with Peanut Oil
>>
>>
>>
>>
>>> Has anyone tried this? It's all I had laying around to start with but I
>>> keep getting a questionable result. Since it was new, I tried the same
>>> recipe for virgin vegetable oil and it didn't really pass the wash test
>>> >
>>> and as soon as it got cold, it turned into sludge. I wish there was
>>> more pictures - not sure if I'm adding too much of something or too
>>> little or what. I'm using some nice equipment (I work for a laboratory
>>> surplus equipment company) such as a lab scale, pH meter, quality
>>> glassware, hotplate stirrer and a 2L reaction vessel. I'm holding the
>>> temperature right on, mixing for 30 minutes, etc. I have 90% KOH and
>>> 99.9% methanol from a local chem distributor. Not sure when I'm doing
>>> wrong, but any advice would be great. I made a 2x75Gal machine that I
>>> am dying to use and the used oil is piling up.
>>>
>>> Also, I don't know if I'm using my pH meter correctly. Can someone give
>>> directions on proper use of one of these?
>>>
>>> If anyone needs any special equipment, just ask. I even have tanks,
>>> etc.
>>>
>>> _______________________________________________
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>>>
>>>
>>>
>>
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