[Biofuel] A Norwegian alchemist
I wish had some good news, Tom - Your persistence is admirable - yours with me even more ... Since successful titration is not based on luck or magic, I still suspect that there is a very simple answer to the problem. Well, everything is a mystery before it becomes science ... My titration no doubt still belongs to the mystery category! I endure because I have spent so much time on this that I simply can't afford to give up. In the meantime I find the correct amount of lye through my series of test batches. Yesterday I hit the bull's eye with a 0,5 liter sample from a 200 liter barrel with palm oil; it passed the wash test and the methanol test - with 6,35 grammes NaOH (titration: 1,9 ml + 3,5 = 5,4 g) and 21,5% methanol. I got hold of all this palm oil (in all 550 liters) before I noticed at JtF that palm oil was difficult, with a high natural content of FFA. (Later on I've found a restaurant with sunflower oil that gives approved results with astoundingly low 3,65 g NaOH). - With regard to the palm oil: I'm planning to scale slowly up - via 3-4 liters and 15 liters to 75 liters. Would you warn me against making biodiesel from oil with that high amounts of FFA - in a one-stage prosess? Should I wait until I can handle the two-stage reaction, or the foolproof? - As for the titration experiment you recommend: Instead of adding drop-by-drop, squirt in the 1.6ml. titration solution into the warm, clear WVO, phenolph, alcohol solution. ... I don't have good news. The mix turns purple and stays purple upon swirling. The temperature of the warm, clear phenolph-alcohol solution is above 40 degrees C. A minute or two after the titration is finished, bubbles of oil appear. Do you have a small, plastic water/juice/sports drink bottle rather than using a shot glass and spoon? I am not sure if I understand what you mean - a very tiny (50 ml ...?) bottle to shake instead of swirling with a spoon? - I find my shot glass quite suitable; it has no stem, but a 1 cm thick bottom, which means it maintaines the temperature once it's got warm (but I wouldn't mind change to something even better). - Attempting to solve this mystery I've also bought a few grammes of new phenolphthalein powder. It wasn't likely that the phenolph was the sinner, but having tested all the likely sources of error, I was transferring into more doubtful zones: The lab where I bought the phenolphthalein in February, belonged to the local waterworks. A couple of months ago the leader of the waterworks was sentenced to 8 years in prison for corruption and misappropriation of funds, and to pay back 12 million dollars(!) to the authorities. I had told the people at the lab that I'd spent an awful lot of time with unsuccessful titration. Could it be that the culture of the whole company was corrupt, and that they had adjusted their pH-meter to show 8,5 when I came there with my purple oil-phenolph solution - to avoid me blaming them for my misery ...? - Of course it couldn't. The new phenplph powder gave exactly the same titration values as the waterwork phenolph solution ... So I'll have to go back to basic once again, checking my procedure step by step: Have I correctly measured out the amount of NaOH/destilled water 5:500 - and then divided 1:9? I'll take a look at that. Best regards Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Tuesday, June 17, 2008 3:21 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, Your titration procedure: 1. Heating and swirling 1 ml palm oil (measured with a 1 ml syringe), 10 ml isopropyl alcohol (10 ml syringe) and 2 drops of 1 % phenolphthalein in a shot glass in hot water bath. 2. Adding the titration solution (0,1% NaOH/distilled water) drop by drop with a 5 ml syringe - while stirring - until the solution turned pink, and stayed pink for 10-15 seconds. - Results: 1,5 and 1,6. It should (as I said) have been 2,65. This is what I have. Not much to take hold of, is it? Everything looks fine. Since successful titration is not based on luck or magic, I still suspect that there is a very simple answer to the problem. About a year ago I got a phone call from a friend I had helped get started making BD. After dozens of successful batches, he had begun to get emulsions and failed quality tests. We went over every detail on the phone then repeated each step he had taken. Unable to resolve the problem, I simply drove over to his house and we discovered a very simple error he was making in titration. Unfortunately I can't drive over to your place, so please bear with me. Why would you consistently get low titration results? Everything you are doing appears to be correct. Your chemicals seem to be high quality
Re: [Biofuel] A Norwegian alchemist
Ove, Your titration procedure: 1. Heating and swirling 1 ml palm oil (measured with a 1 ml syringe), 10 ml isopropyl alcohol (10 ml syringe) and 2 drops of 1 % phenolphthalein in a shot glass in hot water bath. 2. Adding the titration solution (0,1% NaOH/distilled water) drop by drop with a 5 ml syringe - while stirring - until the solution turned pink, and stayed pink for 10-15 seconds. - Results: 1,5 and 1,6. It should (as I said) have been 2,65. This is what I have. Not much to take hold of, is it? Everything looks fine. Since successful titration is not based on luck or magic, I still suspect that there is a very simple answer to the problem. About a year ago I got a phone call from a friend I had helped get started making BD. After dozens of successful batches, he had begun to get emulsions and failed quality tests. We went over every detail on the phone then repeated each step he had taken. Unable to resolve the problem, I simply drove over to his house and we discovered a very simple error he was making in titration. Unfortunately I can't drive over to your place, so please bear with me. Why would you consistently get low titration results? Everything you are doing appears to be correct. Your chemicals seem to be high quality Your measurements look to be right on Your persistence is admirable A thought keeps coming to mind regarding the procedure you follow. Something to consider: WVO will remain dissolved in warm isopropyl alcohol After adding titration solution (99.9% water) the WVO tends to fall out. When I titrate, I am determined to keep the WVO dissolved as titration solution is added - FINISH QUICKLY; my titration solution flows from the syringe; not drop-by- drop - keep the mix warm - swirl the mix as constantly as possible -As the purple color begins to appear I slow the rate at which I add titration solution. I can't help but think that some of the WVO is falling out of solution while you are adding the titration solution drop-by-drop --- artificially low titration results. stayed pink for 10-15 seconds. - Results: 1,5 and 1,6. It should (as I said) have been 2,65. Experiment: If you still have some of the WVO that was successfully converted using 2.65g KOH/L of WVO (rather than the 1.5g and 1.6g KOH that you got from titration) try the following: - Re-titrate it: 10ml Isopropyl alc, 2 drops phenolph, 1ml of the WVO - Heat and swirl (do you have a small, plastic water/juice/sports drink bottle rather than using a shot glass and spoon?) - Have your 5ml (titration solution) syringe filled to 1.6ml and ready to go. Instead of adding drop-by-drop, squirt in the 1.6ml. titration solution into the warm, clear WVO, phenolph, alcohol solution. Does the mix turn purple and stay purple upon swirling? Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Friday, June 13, 2008 6:28 AM Subject: Re: [Biofuel] A Norwegian alchemist Thanks, Tom - also for your generous offer to mail me some phenolphthalein. - But as you say: The phenolphthalein seems good. It is also possible to acquire phenolphthalein powder in Oslo. - As for the solvent: The first phenolphthalein I had, was dissolved in isopropyl alcohol. Question for you: Prior to adding titration solution, is the WVO dissolved in the mix of isopropanol and phenolphthalein? - Is the mix warm and clear? - Kept warm and swirled throughout the titration process? Yes, the WVO is dissolved in the mix of (99,9%) isopropyl alcohol and phenolphthalein, and it is warm and clear and kept swirled throughout the prosess. - Does it matter that I use a metal tea spoon to swirl with? I've been distracted a bit. I don't recall if you ever posted, step-by-step, the procedure and results of a titration. - Not of any special titration. - So I've made two new titrations today - with a palm oil with which I've had successful test batches (passed Wash Test and Methanol Test), using 6,15 g NaOH. It should, in other words, titrate 2,65. This is how I did it: 1. Heating and swirling 1 ml palm oil (measured with a 1 ml syringe), 10 ml isopropyl alcohol (10 ml syringe) and 2 drops of 1 % phenolphthalein in a shot glass in hot water bath. 2. Adding the titration solution (0,1% NaOH/distilled water) drop by drop with a 5 ml syringe - while stirring - until the solution turned pink, and stayed pink for 10-15 seconds. - Results: 1,5 and 1,6. It should (as I said) have been 2,65. This is what I have. Not much to take hold of, is it? Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Thursday, June
Re: [Biofuel] A Norwegian alchemist
Thanks, Tom
- also for your generous offer to mail me some phenolphthalein. - But as
you say: The phenolphthalein seems good.
It is also possible to acquire phenolphthalein powder in Oslo.
- As for the solvent: The first phenolphthalein I had, was dissolved in
isopropyl alcohol.
Question for you:
Prior to adding titration solution, is the WVO dissolved in the mix of
isopropanol and phenolphthalein?
- Is the mix warm and clear?
- Kept warm and swirled throughout the titration process?
Yes, the WVO is dissolved in the mix of (99,9%) isopropyl alcohol and
phenolphthalein, and it is warm and clear and kept swirled throughout the
prosess.
- Does it matter that I use a metal tea spoon to swirl with?
I've been distracted a bit. I don't recall if you ever posted,
step-by-step, the procedure and results of a titration.
- Not of any special titration. - So I've made two new titrations
today - with a palm oil with which I've had successful test batches (passed
Wash Test and Methanol Test), using 6,15 g NaOH. It should, in other words,
titrate 2,65. This is how I did it:
1. Heating and swirling 1 ml palm oil (measured with a 1 ml syringe),
10 ml isopropyl alcohol (10 ml syringe) and 2 drops of 1 % phenolphthalein
in a shot glass in hot water bath.
2. Adding the titration solution (0,1% NaOH/distilled water) drop by
drop with a 5 ml syringe - while stirring - until the solution turned pink,
and stayed pink for 10-15 seconds. - Results: 1,5 and 1,6. It should (as I
said) have been 2,65.
This is what I have. Not much to take hold of, is it?
Ove
- Original Message -
From: Thomas Kelly [EMAIL PROTECTED]
To: sustainablelorgbiofuel@sustainablelists.org
Sent: Thursday, June 12, 2008 1:55 PM
Subject: Re: [Biofuel] A Norwegian alchemist
Ove,
pH at color change = 8.5
The phenolphthalein that I bought at the lab, was solved in isopropyl
alcohol, because they didn't have ethanol.
I dissolve my phenolphthalein in isopropyl alc. as well. It works fine.
Could the isopropyl alcohol and the methanol be the cause of three months
of titration
misery?
I doubt it.
Although I've never used phenolphthalein dissolved in methanol, I don't
think it would make a difference.
Titration: 10ml of 95% isopropanol : 2 drops of phenolphthalein
We use warm isopropanol to dissolve the WVO because oils dissolve in it
better than they do in either ethanol or methanol. We use phenolphthalein as
the indicator because it not only changes color at the appropriate pH, but
because it is soluble in alcohol(s). Both ethanol and methanol dissolve in
isopropanol. It shouldn't matter which alcohol is in the 2 drops of
phenolphthalein that we add.
Question for you:
Prior to adding titration solution, is the WVO dissolved in the mix of
isopropanol and phenolphthalein?
- Is the mix warm and clear?
- Kept warm and swirled throughout the titration process?
If the WVO is allowed to settle out you will get inaccurate (too low)
results.
We seem to have eliminated the possibility that the chemicals are at
fault. (You do use 95% isopropyl alc, not 70%?) Your measurements seem to be
accurate. I can't help but think that there is a very basic flaw in the
procedure.
I've been distracted a bit. I don't recall if you ever posted,
step-by-step, the procedure and results of a titration.
Tom
- Original Message -
From: Ove Steen [EMAIL PROTECTED]
To: sustainablelorgbiofuel@sustainablelists.org
Sent: Monday, June 09, 2008 9:26 AM
Subject: Re: [Biofuel] A Norwegian alchemist
To make a long story short, Tom -
{I've been doing a lot of (more or less systematic) tests since Friday -
among other the one you recommended: ***Try adding 2 drops of
phenolphthalein to 10ml of distilled water. Add titration solution
drop-by-drop until it turns pink/purple. Check mix with pH paper. It should
be about 8***. - The pH paper showed 5-6. - I even have visited the
laboratory where I bought the phenolphthalein, having them measure the above
mentioned purple red solution with their pH meter. Result: 8,5! - But their
pH paper - like mine - indicated 5 or 6!}
- The short story is, that 5 minutes ago I re-read the chapter
'Phenolfthalein' at JtF - where it says that the phenolphthalein is to be
solved in ethanol. The phenolphthalein that I bought at the lab, was solved
in isopropyl alcohol, because they didn't have ethanol. It shouldn't make
any difference, they said. Later, when I encountered all the titration
difficulties, I thought that the isopropanol perhaps might be the sinner.
That's why I changed the phenolphthalein, as I wrote. However - in my mind
ethanol had become methanol. In other words, I got a new solution at the
lab: 1 gram phenolphthalein / 100 ml methanol!
So before I tell you about my week end tests, I must ask you: Could
Re: [Biofuel] A Norwegian alchemist
Ove,
The phenolphthalein seems good pH at color change = 8.5
The phenolphthalein that I bought at the lab, was solved in isopropyl
alcohol, because they didn't have ethanol.
I dissolve my phenolphthalein in isopropyl alc. as well. It works fine.
Could the isopropyl alcohol and the methanol be the cause of three months
of titration
misery?
I doubt it.
Although I've never used phenolphthalein dissolved in methanol, I don't
think it would make a difference.
Titration: 10ml of 95% isopropanol : 2 drops of phenolphthalein
We use warm isopropanol to dissolve the WVO because oils dissolve in it
better than they do in either ethanol or methanol. We use phenolphthalein as
the indicator because it not only changes color at the appropriate pH, but
because it is soluble in alcohol(s). Both ethanol and methanol dissolve in
isopropanol. It shouldn't matter which alcohol is in the 2 drops of
phenolphthalein that we add.
Question for you:
Prior to adding titration solution, is the WVO dissolved in the mix of
isopropanol and phenolphthalein?
- Is the mix warm and clear?
- Kept warm and swirled throughout the titration process?
If the WVO is allowed to settle out you will get inaccurate (too low)
results.
We seem to have eliminated the possibility that the chemicals are at
fault. (You do use 95% isopropyl alc, not 70%?) Your measurements seem to be
accurate. I can't help but think that there is a very basic flaw in the
procedure.
I've been distracted a bit. I don't recall if you ever posted,
step-by-step, the procedure and results of a titration.
Tom
- Original Message -
From: Ove Steen [EMAIL PROTECTED]
To: sustainablelorgbiofuel@sustainablelists.org
Sent: Monday, June 09, 2008 9:26 AM
Subject: Re: [Biofuel] A Norwegian alchemist
To make a long story short, Tom -
{I've been doing a lot of (more or less systematic) tests since Friday -
among other the one you recommended: ***Try adding 2 drops of
phenolphthalein to 10ml of distilled water. Add titration solution
drop-by-drop until it turns pink/purple. Check mix with pH paper. It should
be about 8***. - The pH paper showed 5-6. - I even have visited the
laboratory where I bought the phenolphthalein, having them measure the above
mentioned purple red solution with their pH meter. Result: 8,5! - But their
pH paper - like mine - indicated 5 or 6!}
- The short story is, that 5 minutes ago I re-read the chapter
'Phenolfthalein' at JtF - where it says that the phenolphthalein is to be
solved in ethanol. The phenolphthalein that I bought at the lab, was solved
in isopropyl alcohol, because they didn't have ethanol. It shouldn't make
any difference, they said. Later, when I encountered all the titration
difficulties, I thought that the isopropanol perhaps might be the sinner.
That's why I changed the phenolphthalein, as I wrote. However - in my mind
ethanol had become methanol. In other words, I got a new solution at the
lab: 1 gram phenolphthalein / 100 ml methanol!
So before I tell you about my week end tests, I must ask you: Could the
isopropyl alcohol and the methanol be the cause of three months of titration
misery?
Hopeful regards,
Ove
- Original Message -
From: Thomas Kelly [EMAIL PROTECTED]
To: sustainablelorgbiofuel@sustainablelists.org
Sent: Friday, June 06, 2008 4:15 PM
Subject: Re: [Biofuel] A Norwegian alchemist
Ove,
Sincere thanks, Tom -
You are most welcome.
Let's see if we can straighten out the difficulties with titration.
Each ml of 0.1% titration solution contains .001 g of NaOH.
Each ml of titration solution used on a ml of veg oil corresponds to a
gram of the same caustic per Liter of the same veg oil.
This all works fine if:
Your isopropyl alcohol is neutral.
Today I've been testing the isopropyl alcohol the way you told me: 10
ml
isopropyl alcohol + 2 drops of phenolphthalein - then adding freshly made
titration solution drop by drop. What happens, is: The solution turns
barely
purple on the first drop - but it doesn't stay purple. On drop no 7 it
turns
deeper purple, and stays purple for some time. - What does this tell?
Your isopropyl alcohol is a bit acidic. Some of your titration solution
is being used to neutralize the isopropyl alcohol. This should produce
higher titration values.
But: (From a previous post dated 6/1/08)
The first successful batch with used oil contained 2,5 grammes extra of
NaOH, but the titration indicated only 0,6 grammes.
Titration always gave too low values.
Further: (Same 6/1/08 post)
When I used a pH-paper on an oil-isopropyl alcohol solution that had
turned pink, it showed 5 or 6!
Phenolphthalein should not turn pink until a pH of about 8.2
It is essential that you have good phenolphthalein solution.
This could be the problem as a color change at 5 or 6
Re: [Biofuel] A Norwegian alchemist
To make a long story short, Tom -
{I've been doing a lot of (more or less systematic) tests since Friday -
among other the one you recommended: ***Try adding 2 drops of
phenolphthalein to 10ml of distilled water. Add titration solution
drop-by-drop until it turns pink/purple. Check mix with pH paper. It should
be about 8***. - The pH paper showed 5-6. - I even have visited the
laboratory where I bought the phenolphthalein, having them measure the above
mentioned purple red solution with their pH meter. Result: 8,5! - But their
pH paper - like mine - indicated 5 or 6!}
- The short story is, that 5 minutes ago I re-read the chapter
'Phenolfthalein' at JtF - where it says that the phenolphthalein is to be
solved in ethanol. The phenolphthalein that I bought at the lab, was solved
in isopropyl alcohol, because they didn't have ethanol. It shouldn't make
any difference, they said. Later, when I encountered all the titration
difficulties, I thought that the isopropanol perhaps might be the sinner.
That's why I changed the phenolphthalein, as I wrote. However - in my mind
ethanol had become methanol. In other words, I got a new solution at the
lab: 1 gram phenolphthalein / 100 ml methanol!
So before I tell you about my week end tests, I must ask you: Could the
isopropyl alcohol and the methanol be the cause of three months of titration
misery?
Hopeful regards,
Ove
- Original Message -
From: Thomas Kelly [EMAIL PROTECTED]
To: sustainablelorgbiofuel@sustainablelists.org
Sent: Friday, June 06, 2008 4:15 PM
Subject: Re: [Biofuel] A Norwegian alchemist
Ove,
Sincere thanks, Tom -
You are most welcome.
Let's see if we can straighten out the difficulties with titration.
Each ml of 0.1% titration solution contains .001 g of NaOH.
Each ml of titration solution used on a ml of veg oil corresponds to a
gram of the same caustic per Liter of the same veg oil.
This all works fine if:
Your isopropyl alcohol is neutral.
Today I've been testing the isopropyl alcohol the way you told me: 10
ml
isopropyl alcohol + 2 drops of phenolphthalein - then adding freshly made
titration solution drop by drop. What happens, is: The solution turns
barely
purple on the first drop - but it doesn't stay purple. On drop no 7 it
turns
deeper purple, and stays purple for some time. - What does this tell?
Your isopropyl alcohol is a bit acidic. Some of your titration solution
is being used to neutralize the isopropyl alcohol. This should produce
higher titration values.
But: (From a previous post dated 6/1/08)
The first successful batch with used oil contained 2,5 grammes extra of
NaOH, but the titration indicated only 0,6 grammes.
Titration always gave too low values.
Further: (Same 6/1/08 post)
When I used a pH-paper on an oil-isopropyl alcohol solution that had
turned pink, it showed 5 or 6!
Phenolphthalein should not turn pink until a pH of about 8.2
It is essential that you have good phenolphthalein solution.
This could be the problem as a color change at 5 or 6 would result in the
low titration values you have gotten. (More titration solution would have
been required to achieve the pH of 8.2 we are striving for.)
***Try adding 2 drops of phenolphthalein to 10ml of distilled water. Add
titration solution drop-by-drop until it turns pink/purple. Check mix with
pH paper. It should be about 8.
I have tried to change the phenolphthalein - without luck.
Do you mean you were unable to get a fresh supply of phenolphthalein?
If you are unable to acquire reliable phenolphthalein I would be happy
to mail you some phenolphthalein (powder or solution) so long as it is legal
to do so.
Best to You,
Tom
- Original Message -
From: Ove Steen [EMAIL PROTECTED]
To: sustainablelorgbiofuel@sustainablelists.org
Sent: Friday, June 06, 2008 7:16 AM
Subject: Re: [Biofuel] A Norwegian alchemist
Sincere thanks, Tom -
for your extensive assistance.
- Your questions:
1. Yes, I have succeeded with test batches using new, unused oil - not
on a basis of titration (which, as I said, gives me trouble), but on a
series of test batches on the same principle as Poor man's titation -
circling in the correct amount of lye.
2. Yes, I have done both Jan Warnqvist test and Wash Test.
I also have succeeded with test batches of WVO. They have passed both
the Wash Test and the Methanol Test. - I've been following the same
procedure as with new oil - with a number of batches with different amount
of lye. - It works, but it takes a lot of time.
- Titration:
I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops
of phenolphthalein - but I'm having the same incomprehensible results.
Is this after you made fresh titration solution? (1 g NaOH per Liter
of distilled
Re: [Biofuel] A Norwegian alchemist
Sincere thanks, Tom - for your extensive assistance. - Your questions: 1. Yes, I have succeeded with test batches using new, unused oil - not on a basis of titration (which, as I said, gives me trouble), but on a series of test batches on the same principle as Poor man's titation - circling in the correct amount of lye. 2. Yes, I have done both Jan Warnqvist test and Wash Test. I also have succeeded with test batches of WVO. They have passed both the Wash Test and the Methanol Test. - I've been following the same procedure as with new oil - with a number of batches with different amount of lye. - It works, but it takes a lot of time. - Titration: I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops of phenolphthalein - but I'm having the same incomprehensible results. Is this after you made fresh titration solution? (1 g NaOH per Liter of distilled water) Is your balance accurate to tenths of a gram? Some digital scales are only accurate to whole grams. I'm concerned that your titration solution may be the problem. - Yes, this is with fresh titration solution (5 grammes NaOH in 500 ml distilled water - diluted further 1:9). - I use a 0,01 g electronic balance. Today I've been testing the isopropyl alcohol the way you told me: 10 ml isopropyl alcohol + 2 drops of phenolphtalein - then adding freshly made titration solution drop by drop. What happens, is: The solution turns barely purple on the first drop - but it doesn't stay purple. On drop no 7 it turns deeper purple, and stays purple for some time. - What does this tell? - My failed Wash Tests: I have had both variants - too much soap between the water and BD layer, - and: Emulsion forms, and the separation fails to happen within 30 minutes. Do these Wash Test results tell whether there has been too much or too little lye - or methanol - in the reaction? - Settling time: I always use more than 8 hours, normally12 hours or more. I syphon the BD from the glycerine mix - very carefully. Conclusion so far: My main problem is the tiration. Solving that mystery woud be a breakthrough. With kind regards from a summery Oslo - my WVO melting in the sun - Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Thursday, June 05, 2008 4:12 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, Sorry I'm a bit slow to respond. I'm juggling a number of projects at the moment. It is not unusual to have some problems with test batches. It is also common to achieve success and then run into problems scaling up to larger batch size. It invariably turns out to be a simple mistake that must be corrected or a simple adjustment to the process. The biggest danger is over-thinking. Let's not, for the moment, be concerned with other methods or tricks. Let's get the simplest, tried-and-true method to work, and then you can, if you like, move on to other methods. When you ultimately meet with success you will look back and say: It was all there. The instructions at JtF were all I really needed. First: 0.5L - 1.0L test batches using NEW, UNUSED veg oil. Have you done this?Did you have success? The reason for starting with new, unused veg oil is that you eliminate the need for titration. This allows you to focus on the process. If you achieve a good split, pass the wash test, and the Jan Warnqvist quality test, you are ready to move on to test batches w. used (WVO) veg oil. Success with new, unused veg oil resolves any questions about agitation, temp, quality of caustic, methanol and reaction time. You can proceed knowing that you have these variables under control. Second: 0.5L - 1.0L test batches with used (WVO) oil. Success with step one gives confidence and brings a number of variables under control. Step two (WVO) allows you to focus on titration. It also allows you to see the effect of Free Fatty Acids (FFAs), present in WVO, on soap formation, and hence, on the appearance of the wash tests. Note: (This may make sense now; will help answer one of your questions later) - Little soap should be formed when processing new, unused veg oil. What little soap is produced is due to the inevitable, though small, amount of water in the ingredients. - More soap will be produced when processing WVO due to the presence of FFAs which, in the single stage base method, are converted to soap. *** By starting with new, unused veg oil we not only avoid titration in processing the oil, we minimize soap production which can make for problems in the wash. My questions: 1. Have you succeeded with test batches using new, unused veg oil? 2. -If yes, have you done the solubility in methanol quality test (Jan W. test described at JtF), or only the wash test? You must do both. Together they form the basis
Re: [Biofuel] A Norwegian alchemist
Ove, Sincere thanks, Tom - You are most welcome. Let's see if we can straighten out the difficulties with titration. Each ml of 0.1% titration solution contains .001 g of NaOH. Each ml of titration solution used on a ml of veg oil corresponds to a gram of the same caustic per Liter of the same veg oil. This all works fine if: Your isopropyl alcohol is neutral. Today I've been testing the isopropyl alcohol the way you told me: 10 ml isopropyl alcohol + 2 drops of phenolphthalein - then adding freshly made titration solution drop by drop. What happens, is: The solution turns barely purple on the first drop - but it doesn't stay purple. On drop no 7 it turns deeper purple, and stays purple for some time. - What does this tell? Your isopropyl alcohol is a bit acidic. Some of your titration solution is being used to neutralize the isopropyl alcohol. This should produce higher titration values. But: (From a previous post dated 6/1/08) The first successful batch with used oil contained 2,5 grammes extra of NaOH, but the titration indicated only 0,6 grammes. Titration always gave too low values. Further: (Same 6/1/08 post) When I used a pH-paper on an oil-isopropyl alcohol solution that had turned pink, it showed 5 or 6! Phenolphthalein should not turn pink until a pH of about 8.2 It is essential that you have good phenolphthalein solution. This could be the problem as a color change at 5 or 6 would result in the low titration values you have gotten. (More titration solution would have been required to achieve the pH of 8.2 we are striving for.) ***Try adding 2 drops of phenolphthalein to 10ml of distilled water. Add titration solution drop-by-drop until it turns pink/purple. Check mix with pH paper. It should be about 8. I have tried to change the phenolphthalein - without luck. Do you mean you were unable to get a fresh supply of phenolphthalein? If you are unable to acquire reliable phenolphthalein I would be happy to mail you some phenolphthalein (powder or solution) so long as it is legal to do so. Best to You, Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Friday, June 06, 2008 7:16 AM Subject: Re: [Biofuel] A Norwegian alchemist Sincere thanks, Tom - for your extensive assistance. - Your questions: 1. Yes, I have succeeded with test batches using new, unused oil - not on a basis of titration (which, as I said, gives me trouble), but on a series of test batches on the same principle as Poor man's titation - circling in the correct amount of lye. 2. Yes, I have done both Jan Warnqvist test and Wash Test. I also have succeeded with test batches of WVO. They have passed both the Wash Test and the Methanol Test. - I've been following the same procedure as with new oil - with a number of batches with different amount of lye. - It works, but it takes a lot of time. - Titration: I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops of phenolphthalein - but I'm having the same incomprehensible results. Is this after you made fresh titration solution? (1 g NaOH per Liter of distilled water) Is your balance accurate to tenths of a gram? Some digital scales are only accurate to whole grams. I'm concerned that your titration solution may be the problem. - Yes, this is with fresh titration solution (5 grammes NaOH in 500 ml distilled water - diluted further 1:9). - I use a 0,01 g electronic balance. Today I've been testing the isopropyl alcohol the way you told me: 10 ml isopropyl alcohol + 2 drops of phenolphtalein - then adding freshly made titration solution drop by drop. What happens, is: The solution turns barely purple on the first drop - but it doesn't stay purple. On drop no 7 it turns deeper purple, and stays purple for some time. - What does this tell? - My failed Wash Tests: I have had both variants - too much soap between the water and BD layer, - and: Emulsion forms, and the separation fails to happen within 30 minutes. Do these Wash Test results tell whether there has been too much or too little lye - or methanol - in the reaction? - Settling time: I always use more than 8 hours, normally12 hours or more. I syphon the BD from the glycerine mix - very carefully. Conclusion so far: My main problem is the tiration. Solving that mystery woud be a breakthrough. With kind regards from a summery Oslo - my WVO melting in the sun - Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Thursday, June 05, 2008 4:12 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, Sorry I'm a bit slow to respond. I'm juggling a number of projects at the moment
Re: [Biofuel] A Norwegian alchemist
emulsions *** A real problem arises if you have an incomplete reaction + fail to allow enough settling time (or fail to prevent glycerine from contaminating the BD to be washed). Soaps, glycerine + incomplete reaction -- serious emulsions. How long do you allow the mix to settle? I suggest 8 hours (or more). Do you have an effective way of separating the BD from the settled glycerine mix? Finally: Why is there a high content of water in WWO with a high content of FFA? Hydrogen ions dissociate from the acid portion of FFAs when they are exposed to water. This results in a region of charge on the FFAs. Molecules with regions of charge associate better with water than do molecules that don't have such regions of charge. Implication: - Veg oil at the bottom of a storage tank may have a significantly higher titration (FFAs) than oil at the top. Water and associated FFAs have settled over time. And why is it difficult to get rid of the water? - Is there any other method than boiling it off? In an attempt to use the sludge veg oil from the bottom of my storage tanks I've been experimenting with a method of reducing water from veg oil, and at the same time reducing FFAs in the oil. After we get you settled in making good BD, we can discuss what's involved. The WVO you are using is good enough. It doesn't need any treatment other than letting it settle in the sun. I have some thoughts about your other post, but the answeres depend on whether or not you have done test batches with new, unused veg oil. Best Wishes, Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Wednesday, June 04, 2008 9:52 AM Subject: Re: [Biofuel] A Norwegian alchemist Tom, I had bad luck with this letter: I sent it after only two lines. Here is the rest of it: I have followed your 3 point list: fresh 0,1% solution, I've tested the isopropyl alcohol: pH = 6, and I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops of phenolphtalein - but I'm having the same incomprehensible results. - I'll try to find a chemist who can tell me what I am doing wrong. - May I ask you a couple of other questions? The leader of the laboratory of BVEnergi in Norway, Paul Winson (- a factory that prodused biodiesel from new rapeseed oil until 6 weeks ago, when they went bankrupt because USA is dumping the prices on biodiesel in Europe), recommended me to make as much turbulence as possible during the first 20 minutes of a reaction - as crazy as possible - to break up the molecules. After 20 minutes it was OK to reduce the agitation, he said. - Would you agree in that? Isn't it, in case, also logic to do it this way in (at least) the second stage of the foolproof method (which I haven't practiced)? - Or is this method based upon exactly this (less efficient?) type of turbulence? About settling, - Mike Pelly says: An alternative method is to allow the reactants to sit for at least an hour after mixing while keeping the brew above 100 deg F (38 deg C), which keeps the glycerine semi-liquid (it solidifies below 100 deg F). Then carefully decant the biodiesel. - I suppose this means that a wash test can be performed immediately afterwards? - And that the prosessing time can be shortened down this way also for the two-stage method? I have tried to find information in the mail archive about the visible result in the wast test of too little and too much lye. To me it seems as if there is no obvious distinction. In both cases there is something like skimmed milk + café au lait - and I can't tell wether the reason is too little or too much lye. - Am I right, or is it possible to make a more or less precise diagnosis? Finally: Why is there a high content of water in WWO with a high content of FFA? And why is it difficult to get rid of the water? - Is there any other method than boiling it off? Best regards, Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Monday, June 02, 2008 1:27 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, You wrote I've had serious titration difficulties. .. Titration always gave too low values. I have a couple of suggestions: 1. Prepare fresh titration solution using careful, accurate measurements. If titration solution is not 0.1% NaOH, you will get inaccurate results. 1 gram NaOH per Liter of distilled water 0.1% NaOH titration solution. 2. Test you isopropyl alcohol. Unlikely, but it could be alkaline --- inaccurate titration. 3. Next time you titrate, post the numbers: ml of oil, ml of isopropyl, drops of phenolphthalein, ml of (new) titration solution needed to change color to purple. Good Luck
Re: [Biofuel] A Norwegian alchemist
Thanks Keith, - I was tempted by the fact that NaOH is cheaper to use than KOH - so now I am stuck with a 25 kg sack which I have to use up. It will take approximately 5 years if I drive 15.000 km a year, won't it ... As for the question about the two-stage method: I was asking out of curiosity. The biodiesel subject fascinates me; I am full of questions. - But yes, I do realise that I have to make all the necessary newbie steps; I understand the problem with the increasing number of variables. Kind regards - Ove - Original Message - From: Keith Addison [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Wednesday, June 04, 2008 5:00 PM Subject: Re: [Biofuel] A Norwegian alchemist Hello Ove Why are you using NaOH and not KOH? A question to ask your alchemist friend too. KOH is a better catalyst than NaOH and it's easier to use. Some comments... re turbulence, most of the reaction happens quite quickly (less than 20 minutes), but it will happen anyway, more turbulence might make it happen faster, with less turbulence it might take a bit longer. It's not really important, for optimum results you have to adjust the reaction time to fit a full-scale processor anyway, and it's not the bit at the beginning of the process that matters so much, it's the bit at the end, process completion. IMHO you're still a long way from using the two-stage methods, you'll have problems and you won't know how to deal with them because there'll be too many variables. Focus on producing 1-litre test batches that pass the quality checks using the single-stage base method. Depending on your oil supply, it might be all you ever need. Best Keith Tom, I had bad luck with this letter: I sent it after only two lines. Here is the rest of it: I have followed your 3 point list: fresh 0,1% solution, I've tested the isopropyl alcohol: pH = 6, and I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops of phenolphtalein - but I'm having the same incomprehensible results. - I'll try to find a chemist who can tell me what I am doing wrong. - May I ask you a couple of other questions? The leader of the laboratory of BVEnergi in Norway, Paul Winson (- a factory that prodused biodiesel from new rapeseed oil until 6 weeks ago, when they went bankrupt because USA is dumping the prices on biodiesel in Europe), recommended me to make as much turbulence as possible during the first 20 minutes of a reaction - as crazy as possible - to break up the molecules. After 20 minutes it was OK to reduce the agitation, he said. - Would you agree in that? Isn't it, in case, also logic to do it this way in (at least) the second stage of the foolproof method (which I haven't practiced)? - Or is this method based upon exactly this (less efficient?) type of turbulence? About settling, - Mike Pelly says: An alternative method is to allow the reactants to sit for at least an hour after mixing while keeping the brew above 100 deg F (38 deg C), which keeps the glycerine semi-liquid (it solidifies below 100 deg F). Then carefully decant the biodiesel. - I suppose this means that a wash test can be performed immediately afterwards? - And that the prosessing time can be shortened down this way also for the two-stage method? I have tried to find information in the mail archive about the visible result in the wast test of too little and too much lye. To me it seems as if there is no obvious distinction. In both cases there is something like skimmed milk + café au lait - and I can't tell wether the reason is too little or too much lye. - Am I right, or is it possible to make a more or less precise diagnosis? Finally: Why is there a high content of water in WWO with a high content of FFA? And why is it difficult to get rid of the water? - Is there any other method than boiling it off? Best regards, Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Monday, June 02, 2008 1:27 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, You wrote I've had serious titration difficulties. .. Titration always gave too low values. I have a couple of suggestions: 1. Prepare fresh titration solution using careful, accurate measurements. If titration solution is not 0.1% NaOH, you will get inaccurate results. 1 gram NaOH per Liter of distilled water 0.1% NaOH titration solution. 2. Test you isopropyl alcohol. Unlikely, but it could be alkaline --- inaccurate titration. 3. Next time you titrate, post the numbers: ml of oil, ml of isopropyl, drops of phenolphthalein, ml of (new) titration solution needed to change color to purple. Good Luck, Tom - Original Message - From: Ove Steen [EMAIL PROTECTED
Re: [Biofuel] A Norwegian alchemist
Tom, I have followed your 3 point list: fresh 0,1% solution, I've tested the isopropyl alcohol: pH = 6, and I'm using the recipe - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Monday, June 02, 2008 1:27 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, You wrote I've had serious titration difficulties. .. Titration always gave too low values. I have a couple of suggestions: 1. Prepare fresh titration solution using careful, accurate measurements. If titration solution is not 0.1% NaOH, you will get inaccurate results. 1 gram NaOH per Liter of distilled water 0.1% NaOH titration solution. 2. Test you isopropyl alcohol. Unlikely, but it could be alkaline --- inaccurate titration. 3. Next time you titrate, post the numbers: ml of oil, ml of isopropyl, drops of phenolphthalein, ml of (new) titration solution needed to change color to purple. Good Luck, Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Sunday, June 01, 2008 8:42 AM Subject: Re: [Biofuel] A Norwegian alchemist Thanks, Tom - Your answer was, perhaps, as I had feared: FFA's in the biodiesel. - I've been on the point of chosing his method, because I've had serious titration difficulties. After about 40 test batches I finally succeeded in making biodiesel that passed the wash test - not because of the titration, but in spite of it: The first successful batch with used oil contained 2,5 grammes extra of NaOH, but the titration indicated only 0,6 grammes. When I used a pH-paper on an oil-isopropyl alcohol solution that had turned pink, it showed 5 or 6! I have tried to change the phenolphthalein - without luck. What am I doing wrong? - My answer to the problems has been a series of test batches. I've also tried Poor man's titration, but the amount of glycerin cocktail has varied so little that I haven't dared trusting the results. And I made a strange experience: The first batch that passed the wash test (0,5 litre sunflower oil, 6,0 grammes pr. litre of NaOH), contained 70 ml glycerin cocktail, while batches that didn't pass the test - with respectively 5,75 grammes - 6,25 gr. - 6,50 gr. - 7,0 gr. - 7,5 gr. and 8,0 grammes of NaOH, contained 70 - 77,5 - 95 - 85 and 91 ml of glycerin! Very confusing to a newbie. - Any explanation? Anyhow - I have to learn titration - . I've sent your e-mail to the man with the 'foolproof ' recipe. I think he'll come up with an answer. - He was incautious with a 200 litre batch some time ago - water in the oil - and is out of biodiesel at the moment, but he'll make more in the course of a month or so, he says - and make a wash test and a methanol test. I'll let you know the results. - Thanks again, Tom. Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Saturday, May 31, 2008 2:07 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, Just a thought regarding the use of acid in, or prior to, the first wash. There is a danger of splitting the soaps produced during processing into Free Fatty Acids (FFAs) and a water soluble salt. While this will effectively remove soaps and hence make washing easier, the FFAs produced will remain with the biodiesel. This is not a problem if your intent is to make biodiesel to be burned in an oil-fired boiler/furnace/water heater, but, I've been told, not so good on automobile engines. If he uses NaOH as his caustic and hydrochloric acid (HCl) in the wash, the water soluble salt will be sodium chloride (NaCl = table salt). Sulfuric acid (H2SO4) will yield sodium sulfate. Having a degree in chemistry, he should be no stranger to titration. It would allow him to determine the correct amount of caustic for each batch. The one size fits all concept no titration, 7 grammes of NaOH regardless of type of oil, strikes me as sloppy chemistry and wasteful. Adding acid to the wash strikes me as a way (possibly) of dealing with a problem that could have been avoided in the first place. The thought that comes to mind is that he is developing a proceedure that anyone can follow. No need to understand the process, just follow the recipe. Biodiesel the easy way vs. JtF and the biofuel list: biodiesel the right way. I could be wrong. I'm just a small-time homebrewer w/o any degrees in chemistry. I would be interested in the results of a quality test of his finished product, as described at JtF. If soaps are being split by the acid, the FFAs produced will be in the BD. FFAs are not very soluble in methanol residue in quality test. Tom - Original Message - From
Re: [Biofuel] A Norwegian alchemist
Tom, I had bad luck with this letter: I sent it after only two lines. Here is the rest of it: I have followed your 3 point list: fresh 0,1% solution, I've tested the isopropyl alcohol: pH = 6, and I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops of phenolphtalein - but I'm having the same incomprehensible results. - I'll try to find a chemist who can tell me what I am doing wrong. - May I ask you a couple of other questions? The leader of the laboratory of BVEnergi in Norway, Paul Winson (- a factory that prodused biodiesel from new rapeseed oil until 6 weeks ago, when they went bankrupt because USA is dumping the prices on biodiesel in Europe), recommended me to make as much turbulence as possible during the first 20 minutes of a reaction - as crazy as possible - to break up the molecules. After 20 minutes it was OK to reduce the agitation, he said. - Would you agree in that? Isn't it, in case, also logic to do it this way in (at least) the second stage of the foolproof method (which I haven't practiced)? - Or is this method based upon exactly this (less efficient?) type of turbulence? About settling, - Mike Pelly says: An alternative method is to allow the reactants to sit for at least an hour after mixing while keeping the brew above 100 deg F (38 deg C), which keeps the glycerine semi-liquid (it solidifies below 100 deg F). Then carefully decant the biodiesel. - I suppose this means that a wash test can be performed immediately afterwards? - And that the prosessing time can be shortened down this way also for the two-stage method? I have tried to find information in the mail archive about the visible result in the wast test of too little and too much lye. To me it seems as if there is no obvious distinction. In both cases there is something like skimmed milk + café au lait - and I can't tell wether the reason is too little or too much lye. - Am I right, or is it possible to make a more or less precise diagnosis? Finally: Why is there a high content of water in WWO with a high content of FFA? And why is it difficult to get rid of the water? - Is there any other method than boiling it off? Best regards, Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Monday, June 02, 2008 1:27 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, You wrote I've had serious titration difficulties. .. Titration always gave too low values. I have a couple of suggestions: 1. Prepare fresh titration solution using careful, accurate measurements. If titration solution is not 0.1% NaOH, you will get inaccurate results. 1 gram NaOH per Liter of distilled water 0.1% NaOH titration solution. 2. Test you isopropyl alcohol. Unlikely, but it could be alkaline --- inaccurate titration. 3. Next time you titrate, post the numbers: ml of oil, ml of isopropyl, drops of phenolphthalein, ml of (new) titration solution needed to change color to purple. Good Luck, Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Sunday, June 01, 2008 8:42 AM Subject: Re: [Biofuel] A Norwegian alchemist Thanks, Tom - Your answer was, perhaps, as I had feared: FFA's in the biodiesel. - I've been on the point of chosing his method, because I've had serious titration difficulties. After about 40 test batches I finally succeeded in making biodiesel that passed the wash test - not because of the titration, but in spite of it: The first successful batch with used oil contained 2,5 grammes extra of NaOH, but the titration indicated only 0,6 grammes. When I used a pH-paper on an oil-isopropyl alcohol solution that had turned pink, it showed 5 or 6! I have tried to change the phenolphthalein - without luck. What am I doing wrong? - My answer to the problems has been a series of test batches. I've also tried Poor man's titration, but the amount of glycerin cocktail has varied so little that I haven't dared trusting the results. And I made a strange experience: The first batch that passed the wash test (0,5 litre sunflower oil, 6,0 grammes pr. litre of NaOH), contained 70 ml glycerin cocktail, while batches that didn't pass the test - with respectively 5,75 grammes - 6,25 gr. - 6,50 gr. - 7,0 gr. - 7,5 gr. and 8,0 grammes of NaOH, contained 70 - 77,5 - 95 - 85 and 91 ml of glycerin! Very confusing to a newbie. - Any explanation? Anyhow - I have to learn titration - . I've sent your e-mail to the man with the 'foolproof ' recipe. I think he'll come up with an answer. - He was incautious with a 200 litre batch some time ago - water in the oil - and is out of biodiesel at the moment, but he'll make more in the course
Re: [Biofuel] A Norwegian alchemist
Hello Ove Why are you using NaOH and not KOH? A question to ask your alchemist friend too. KOH is a better catalyst than NaOH and it's easier to use. Some comments... re turbulence, most of the reaction happens quite quickly (less than 20 minutes), but it will happen anyway, more turbulence might make it happen faster, with less turbulence it might take a bit longer. It's not really important, for optimum results you have to adjust the reaction time to fit a full-scale processor anyway, and it's not the bit at the beginning of the process that matters so much, it's the bit at the end, process completion. IMHO you're still a long way from using the two-stage methods, you'll have problems and you won't know how to deal with them because there'll be too many variables. Focus on producing 1-litre test batches that pass the quality checks using the single-stage base method. Depending on your oil supply, it might be all you ever need. Best Keith Tom, I had bad luck with this letter: I sent it after only two lines. Here is the rest of it: I have followed your 3 point list: fresh 0,1% solution, I've tested the isopropyl alcohol: pH = 6, and I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops of phenolphtalein - but I'm having the same incomprehensible results. - I'll try to find a chemist who can tell me what I am doing wrong. - May I ask you a couple of other questions? The leader of the laboratory of BVEnergi in Norway, Paul Winson (- a factory that prodused biodiesel from new rapeseed oil until 6 weeks ago, when they went bankrupt because USA is dumping the prices on biodiesel in Europe), recommended me to make as much turbulence as possible during the first 20 minutes of a reaction - as crazy as possible - to break up the molecules. After 20 minutes it was OK to reduce the agitation, he said. - Would you agree in that? Isn't it, in case, also logic to do it this way in (at least) the second stage of the foolproof method (which I haven't practiced)? - Or is this method based upon exactly this (less efficient?) type of turbulence? About settling, - Mike Pelly says: An alternative method is to allow the reactants to sit for at least an hour after mixing while keeping the brew above 100 deg F (38 deg C), which keeps the glycerine semi-liquid (it solidifies below 100 deg F). Then carefully decant the biodiesel. - I suppose this means that a wash test can be performed immediately afterwards? - And that the prosessing time can be shortened down this way also for the two-stage method? I have tried to find information in the mail archive about the visible result in the wast test of too little and too much lye. To me it seems as if there is no obvious distinction. In both cases there is something like skimmed milk + café au lait - and I can't tell wether the reason is too little or too much lye. - Am I right, or is it possible to make a more or less precise diagnosis? Finally: Why is there a high content of water in WWO with a high content of FFA? And why is it difficult to get rid of the water? - Is there any other method than boiling it off? Best regards, Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Monday, June 02, 2008 1:27 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, You wrote I've had serious titration difficulties. .. Titration always gave too low values. I have a couple of suggestions: 1. Prepare fresh titration solution using careful, accurate measurements. If titration solution is not 0.1% NaOH, you will get inaccurate results. 1 gram NaOH per Liter of distilled water 0.1% NaOH titration solution. 2. Test you isopropyl alcohol. Unlikely, but it could be alkaline --- inaccurate titration. 3. Next time you titrate, post the numbers: ml of oil, ml of isopropyl, drops of phenolphthalein, ml of (new) titration solution needed to change color to purple. Good Luck, Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Sunday, June 01, 2008 8:42 AM Subject: Re: [Biofuel] A Norwegian alchemist Thanks, Tom - Your answer was, perhaps, as I had feared: FFA's in the biodiesel. - I've been on the point of chosing his method, because I've had serious titration difficulties. After about 40 test batches I finally succeeded in making biodiesel that passed the wash test - not because of the titration, but in spite of it: The first successful batch with used oil contained 2,5 grammes extra of NaOH, but the titration indicated only 0,6 grammes. When I used a pH-paper on an oil-isopropyl alcohol solution that had turned pink, it showed 5 or 6! I have tried to change
Re: [Biofuel] A Norwegian alchemist
Ove, You wrote I've had serious titration difficulties. .. Titration always gave too low values. I have a couple of suggestions: 1. Prepare fresh titration solution using careful, accurate measurements. If titration solution is not 0.1% NaOH, you will get inaccurate results. 1 gram NaOH per Liter of distilled water 0.1% NaOH titration solution. 2. Test you isopropyl alcohol. Unlikely, but it could be alkaline --- inaccurate titration. 3. Next time you titrate, post the numbers: ml of oil, ml of isopropyl, drops of phenolphthalein, ml of (new) titration solution needed to change color to purple. Good Luck, Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Sunday, June 01, 2008 8:42 AM Subject: Re: [Biofuel] A Norwegian alchemist Thanks, Tom - Your answer was, perhaps, as I had feared: FFA's in the biodiesel. - I've been on the point of chosing his method, because I've had serious titration difficulties. After about 40 test batches I finally succeeded in making biodiesel that passed the wash test - not because of the titration, but in spite of it: The first successful batch with used oil contained 2,5 grammes extra of NaOH, but the titration indicated only 0,6 grammes. When I used a pH-paper on an oil-isopropyl alcohol solution that had turned pink, it showed 5 or 6! I have tried to change the phenolphthalein - without luck. What am I doing wrong? - My answer to the problems has been a series of test batches. I've also tried Poor man's titration, but the amount of glycerin cocktail has varied so little that I haven't dared trusting the results. And I made a strange experience: The first batch that passed the wash test (0,5 litre sunflower oil, 6,0 grammes pr. litre of NaOH), contained 70 ml glycerin cocktail, while batches that didn't pass the test - with respectively 5,75 grammes - 6,25 gr. - 6,50 gr. - 7,0 gr. - 7,5 gr. and 8,0 grammes of NaOH, contained 70 - 77,5 - 95 - 85 and 91 ml of glycerin! Very confusing to a newbie. - Any explanation? Anyhow - I have to learn titration - . I've sent your e-mail to the man with the 'foolproof ' recipe. I think he'll come up with an answer. - He was incautious with a 200 litre batch some time ago - water in the oil - and is out of biodiesel at the moment, but he'll make more in the course of a month or so, he says - and make a wash test and a methanol test. I'll let you know the results. - Thanks again, Tom. Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Saturday, May 31, 2008 2:07 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, Just a thought regarding the use of acid in, or prior to, the first wash. There is a danger of splitting the soaps produced during processing into Free Fatty Acids (FFAs) and a water soluble salt. While this will effectively remove soaps and hence make washing easier, the FFAs produced will remain with the biodiesel. This is not a problem if your intent is to make biodiesel to be burned in an oil-fired boiler/furnace/water heater, but, I've been told, not so good on automobile engines. If he uses NaOH as his caustic and hydrochloric acid (HCl) in the wash, the water soluble salt will be sodium chloride (NaCl = table salt). Sulfuric acid (H2SO4) will yield sodium sulfate. Having a degree in chemistry, he should be no stranger to titration. It would allow him to determine the correct amount of caustic for each batch. The one size fits all concept no titration, 7 grammes of NaOH regardless of type of oil, strikes me as sloppy chemistry and wasteful. Adding acid to the wash strikes me as a way (possibly) of dealing with a problem that could have been avoided in the first place. The thought that comes to mind is that he is developing a proceedure that anyone can follow. No need to understand the process, just follow the recipe. Biodiesel the easy way vs. JtF and the biofuel list: biodiesel the right way. I could be wrong. I'm just a small-time homebrewer w/o any degrees in chemistry. I would be interested in the results of a quality test of his finished product, as described at JtF. If soaps are being split by the acid, the FFAs produced will be in the BD. FFAs are not very soluble in methanol residue in quality test. Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Friday, May 30, 2008 10:50 AM Subject: [Biofuel] A Norwegian alchemist Hi all, I have an aquaintance. He is making biodiesel this way: no titration, 7 grammes of NaOH regardless of type of oil, 20% methanol, 12 hours processing time, 40 degrees Celsius. Having disposed of the glycerol
[Biofuel] A Norwegian alchemist
Hi all, I have an aquaintance. He is making biodiesel this way: no titration, 7 grammes of NaOH regardless of type of oil, 20% methanol, 12 hours processing time, 40 degrees Celsius. Having disposed of the glycerol, he brings the pH down to 7 with hydrochloric acid (H2SO4), followed by bubble washing and drying - and that's that. No wash test, never any washing problems. It sounds wonderful, but what's wrong with it? - He's got a degree in chemistry; I am a newbie and can't follow his arguments. - Does he really succeed to disguise processing problems this way - every time? What does H2S04 do with his surplus of NaOH? - Can somebody tell me how to arrest this alchemist? Ove -- next part -- An HTML attachment was scrubbed... URL: /pipermail/attachments/20080530/cd1e56c7/attachment.html ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/sustainablelorgbiofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (70,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
