Re: [Biofuel] tirating a virgin oil
Jan, You wrote: The limit of FFA for a flawless trans-esterification is drawn at 5mg KOH/g of oil. Any value above will demand pre-treatment of the oil. I have been blending the WVO I collect - titration of 2 - 3 g of 90%KOH/L. I recently ran a 76L batch of poor quality WVO . It titrated at 5.5g of 90%KOH/L. For the first time in months, the BD I produced failed the methanol quality test not bad, but there were tiny buggers that did not dissolve. I have been troubled by the failed test. I have never used WVO that titrated above 4g 90% KOH/L. 1. Is it reasonable assume that the failure to make quality BD was due to the poor quality of the WVO I used? 2. What pre-treatment would be appropriate? Tom - Original Message - From: Jan Warnqvist [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Monday, August 21, 2006 10:39 AM Subject: Re: [Biofuel] tirating a virgin oil Hello Emre, Rafal et al. I have to say that I partially disagree with some of your statements. The limit of FFA for a flawless trans-esterification is drawn at 5mg KOH/g of oil. Any value above will demand pre-treatment of the oil. It is always important to check the water content, which should be below 0,5%. Try to get hold of a water-in-oil test kit for quick determination. If we are talking about the EN standard, it is always necessary to process the oil/catalyst/methanol mix for 90 minutes to obtain the right values for tri- di- and monoglycerides. And - this assumes that you have correct stochiometric conditions and no methanol losses during processing. As for the phophatides and the chlorophyll compounds, my experience is that these are not very important for the processing result, unless the values of these are extremely high (thousands of ppms). If so, the oil is usually very dark. Totally refined oil, on the other hand, may have preservatives added, and some of these will eat catalyst. So, good oil quality is a tricky thing. Best of luck to you ! Jan Warnqvist AGERATEC AB ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
Hello Tom. Yes, it is likely that the high FFA content of the oil caused you problems with the methanol test. But, the water content is also important. You should get yourself a water test kit. One way of pre-treatment is to do a two-step process. After the first alkaline step, take off the glycerol and process the oil/ester with methanol and sulphuric acid as catalyst. This will give you a very high ester content. The amount of acid added has to be calculated upon the original FFA value, of course. With best regards Jan Warnqvist AGERATEC AB + 46 554 201 89 +46 70 499 38 45 - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Tuesday, August 22, 2006 7:35 PM Subject: Re: [Biofuel] tirating a virgin oil Jan, You wrote: The limit of FFA for a flawless trans-esterification is drawn at 5mg KOH/g of oil. Any value above will demand pre-treatment of the oil. I have been blending the WVO I collect - titration of 2 - 3 g of 90%KOH/L. I recently ran a 76L batch of poor quality WVO . It titrated at 5.5g of 90%KOH/L. For the first time in months, the BD I produced failed the methanol quality test not bad, but there were tiny buggers that did not dissolve. I have been troubled by the failed test. I have never used WVO that titrated above 4g 90% KOH/L. 1. Is it reasonable assume that the failure to make quality BD was due to the poor quality of the WVO I used? 2. What pre-treatment would be appropriate? Tom - Original Message - From: Jan Warnqvist [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Monday, August 21, 2006 10:39 AM Subject: Re: [Biofuel] tirating a virgin oil Hello Emre, Rafal et al. I have to say that I partially disagree with some of your statements. The limit of FFA for a flawless trans-esterification is drawn at 5mg KOH/g of oil. Any value above will demand pre-treatment of the oil. It is always important to check the water content, which should be below 0,5%. Try to get hold of a water-in-oil test kit for quick determination. If we are talking about the EN standard, it is always necessary to process the oil/catalyst/methanol mix for 90 minutes to obtain the right values for tri- di- and monoglycerides. And - this assumes that you have correct stochiometric conditions and no methanol losses during processing. As for the phophatides and the chlorophyll compounds, my experience is that these are not very important for the processing result, unless the values of these are extremely high (thousands of ppms). If so, the oil is usually very dark. Totally refined oil, on the other hand, may have preservatives added, and some of these will eat catalyst. So, good oil quality is a tricky thing. Best of luck to you ! Jan Warnqvist AGERATEC AB ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
Hi Rafal, If it is virgin oil from the supermarket, you should not worry about water. I had the same problem in my early batches, and I think it is the lye. do some additional test batches with more and more lye. This eay you have an idea and a feel for the process. What you should look for is a perfect wash test. Increase the lye in the batch until you can shake the hell out of it in the wash test and still get perfect separation within minutes. This is what I would be doing. Kind reg. Andrew - Original Message - From: EMRE ELMAS [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Sunday, August 20, 2006 10:15 PM Subject: Re: [Biofuel] tirating a virgin oil Dear Rafal, First of all, as long as you use cheap oil you should always be prepared to deal with much more FFA and water than it should normally contain. I think your emulsion problem occurs as a result of highly contained water. If that is the problem you should first dry the oil then process the reaction. Also if you use crude oil you should be very careful about the chemicals, such as lesitine, in the oil. So always try to use degummed oil, if you have to process crude oil. Another thing is, as you probably know, approximately 95 - 97 % of the reaction is completed in the first 35 minutes, so you do not have to wait for 2 hours. Also the alcohol boils at 65 C and the closer you get to that point, the more alcohol you will lose at the time you need it the most for the reaction. This prevents you to complete the reaction 100 %. As I mentioned above if you just watch the content of water and the other impurities in the oil you will be fine. Hopefully the information works for you. I am looking forward to hear from you soon. Best wishes, Emre ELMAS Mobile: +90 533 517 72 45 From: Rafal Szczesniak [EMAIL PROTECTED] Reply-To: biofuel@sustainablelists.org To: biofuel@sustainablelists.org Subject: [Biofuel] tirating a virgin oil Date: Sun, 20 Aug 2006 19:31:26 +0200 Hi, Recently I've came through problems with testing a cheap virgin oil in my test processor which every time ended up with incomplete reactions (emulsion problems). I did make the process longer (2 hours) and at higher temperature (60-63 degC) - still nothing, though by product separation is very nice. Today, I tried to titrate the oil and - to my surprise - it took 0.925ml of KOH solution. This was my first experience with titration, so I can also tell that the phenolophtalein solution turned pale (but noticable) magenta for about 15 secs (as described at JtF) after 0.925ml. After adding 1.05ml the colour got more intensive for longer time. My main question is - is it normal in case of cheap oils ? I suppose they contain (as other oils) some amount of FFAs, but so much ? Additional matter is whether I got titration right. I mean, interpreting the colours. I'm running out of ideas what could be wrong in the process, so any help is appreciated. -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ _ Don't just search. Find. Check out the new MSN Search! http://search.msn.click-url.com/go/onm00200636ave/direct/01/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
Rafal, 1 - 2L test batches w. virgin oil . Good 99% pure KOH V. Good (If you are concerned about the purity and have NaOH of known purity you can test the KOH) Temp and agitation also sound good. If there is water in the methanol you will make more soap (emulsion) and there will be less methanol --- incomplete reaction (emulsion). As I understand it, you have done test batches w virgin oil and have gotten unsatisfactory results emulsions upon washing. You are concerned about incomplete reactions. Question #1: Are you careful to exclude the glycerine byproduct from the wash? Question #2: The oil titrated at 0.925 ml of .99KOH.. This is significant. Have you run a batch with an additional .9 - 1.0 g KOH/L you got from titration? 3.5g 100%NaOH/L of oil = 4.9 g 100%KOH/L of oil Add 0.9 - 1.0 g of the KOH (from titration) you would be using 5.8 - 5.9 g of KOH/L of oil. This additional .9 -1.0 g represents an increase of 18 - 20% over the amount used for virgin oil w/o FFAs. When you consider that your KOH may be less than 99% pure, the amount needed would be even higher. This could very well be the cause of the incomplete reaction. Treat the virgin oil as if it was WVO. Include your titration results in the amount of KOH to be added and run a batch exactly as you have before. Let us know how it worked out and we'll proceed from there. Of course you could go out and buy some high quality veg oil that titrates zero, but then we would not get the answer to the puzzle. Best to you, Tom - Original Message - From: Rafal Szczesniak [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Sunday, August 20, 2006 7:22 PM Subject: Re: [Biofuel] tirating a virgin oil On Sun, Aug 20, 2006 at 06:29:51PM -0400, Thomas Kelly wrote: Rafal, I assume you are doing 1L test batches? Correct me if I'm wrong. Yes. Actually these are 1 or 2l test batches. For agitation I use a small water pump originally designed for larger aquaria and also recently used in water cooling systems for PCs. Manufacturer says it's capacity is 700 liters per hour. Even considering higher viscosity of oil it should be enough for 5l testing container. Do you think it is ? I can provide some pictures if it helps (I've done a bit of documentation). Do you know the purity of the KOH you are using? Yes, it's 99% pure from chemical supplier, though I've noticed it's a little bit calcinated (some flakes are too white, in my opinion). I have also tried NaOH (same purity) before with the same result. I have heard of virgin oil containing some FFA. I have no experience with such oil. It's probably normal, as it sounds impossible to make fresh oil with absolutely no FFAs. The question is - what amount is 'normal' and what is definately not ? -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
Hello Emre, Rafal et al. I have to say that I partially disagree with some of your statements. The limit of FFA for a flawless trans-esterification is drawn at 5mg KOH/g of oil. Any value above will demand pre-treatment of the oil. It is always important to check the water content, which should be below 0,5%. Try to get hold of a water-in-oil test kit for quick determination. If we are talking about the EN standard, it is always necessary to process the oil/catalyst/methanol mix for 90 minutes to obtain the right values for tri- di- and monoglycerides. And - this assumes that you have correct stochiometric conditions and no methanol losses during processing. As for the phophatides and the chlorophyll compounds, my experience is that these are not very important for the processing result, unless the values of these are extremely high (thousands of ppms). If so, the oil is usually very dark. Totally refined oil, on the other hand, may have preservatives added, and some of these will eat catalyst. So, good oil quality is a tricky thing. Best of luck to you ! Jan Warnqvist AGERATEC AB + 46 554 201 89 +46 70 499 38 45 - Original Message - From: EMRE ELMAS [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Sunday, August 20, 2006 10:15 PM Subject: Re: [Biofuel] tirating a virgin oil Dear Rafal, First of all, as long as you use cheap oil you should always be prepared to deal with much more FFA and water than it should normally contain. I think your emulsion problem occurs as a result of highly contained water. If that is the problem you should first dry the oil then process the reaction. Also if you use crude oil you should be very careful about the chemicals, such as lesitine, in the oil. So always try to use degummed oil, if you have to process crude oil. Another thing is, as you probably know, approximately 95 - 97 % of the reaction is completed in the first 35 minutes, so you do not have to wait for 2 hours. Also the alcohol boils at 65 C and the closer you get to that point, the more alcohol you will lose at the time you need it the most for the reaction. This prevents you to complete the reaction 100 %. As I mentioned above if you just watch the content of water and the other impurities in the oil you will be fine. Hopefully the information works for you. I am looking forward to hear from you soon. Best wishes, Emre ELMAS Mobile: +90 533 517 72 45 From: Rafal Szczesniak [EMAIL PROTECTED] Reply-To: biofuel@sustainablelists.org To: biofuel@sustainablelists.org Subject: [Biofuel] tirating a virgin oil Date: Sun, 20 Aug 2006 19:31:26 +0200 Hi, Recently I've came through problems with testing a cheap virgin oil in my test processor which every time ended up with incomplete reactions (emulsion problems). I did make the process longer (2 hours) and at higher temperature (60-63 degC) - still nothing, though by product separation is very nice. Today, I tried to titrate the oil and - to my surprise - it took 0.925ml of KOH solution. This was my first experience with titration, so I can also tell that the phenolophtalein solution turned pale (but noticable) magenta for about 15 secs (as described at JtF) after 0.925ml. After adding 1.05ml the colour got more intensive for longer time. My main question is - is it normal in case of cheap oils ? I suppose they contain (as other oils) some amount of FFAs, but so much ? Additional matter is whether I got titration right. I mean, interpreting the colours. I'm running out of ideas what could be wrong in the process, so any help is appreciated. -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ _ Don't just search. Find. Check out the new MSN Search! http://search.msn.click-url.com/go/onm00200636ave/direct/01/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org
Re: [Biofuel] tirating a virgin oil
Jan, With well-deserved respect to you Rafal's oil titrated to .925 - 1.0 mgKOH/g of oil. This is far below the 5mgKOH/L of oil that you mention as the limit of FFA for flawless a trans-esterification. It is, however, a significant enough amount that, if excluded, could contribute to an incomplete reaction. If we are talking about the EN standard, it is always necessary to process the oil/catalyst/methanol mix for 90 minutes to obtain the right values for tri- di- and monoglycerides. And - this assumes that you have correct stochiometric conditions and no methanol losses during processing. While it is very difficult to achieve a complete reaction on 1L and 2L batches w/o laboratory conditions, it is possible to produce BD that will at least pass the wash test. From this starting point one can scale up slowly sealed containers . tweaking the process to produce quality fuel. Tom - Original Message - From: Jan Warnqvist [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Monday, August 21, 2006 10:39 AM Subject: Re: [Biofuel] tirating a virgin oil Hello Emre, Rafal et al. I have to say that I partially disagree with some of your statements. The limit of FFA for a flawless trans-esterification is drawn at 5mg KOH/g of oil. Any value above will demand pre-treatment of the oil. It is always important to check the water content, which should be below 0,5%. Try to get hold of a water-in-oil test kit for quick determination. If we are talking about the EN standard, it is always necessary to process the oil/catalyst/methanol mix for 90 minutes to obtain the right values for tri- di- and monoglycerides. And - this assumes that you have correct stochiometric conditions and no methanol losses during processing. As for the phophatides and the chlorophyll compounds, my experience is that these are not very important for the processing result, unless the values of these are extremely high (thousands of ppms). If so, the oil is usually very dark. Totally refined oil, on the other hand, may have preservatives added, and some of these will eat catalyst. So, good oil quality is a tricky thing. Best of luck to you ! Jan Warnqvist AGERATEC AB + 46 554 201 89 +46 70 499 38 45 - Original Message - From: EMRE ELMAS [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Sunday, August 20, 2006 10:15 PM Subject: Re: [Biofuel] tirating a virgin oil Dear Rafal, First of all, as long as you use cheap oil you should always be prepared to deal with much more FFA and water than it should normally contain. I think your emulsion problem occurs as a result of highly contained water. If that is the problem you should first dry the oil then process the reaction. Also if you use crude oil you should be very careful about the chemicals, such as lesitine, in the oil. So always try to use degummed oil, if you have to process crude oil. Another thing is, as you probably know, approximately 95 - 97 % of the reaction is completed in the first 35 minutes, so you do not have to wait for 2 hours. Also the alcohol boils at 65 C and the closer you get to that point, the more alcohol you will lose at the time you need it the most for the reaction. This prevents you to complete the reaction 100 %. As I mentioned above if you just watch the content of water and the other impurities in the oil you will be fine. Hopefully the information works for you. I am looking forward to hear from you soon. Best wishes, Emre ELMAS Mobile: +90 533 517 72 45 From: Rafal Szczesniak [EMAIL PROTECTED] Reply-To: biofuel@sustainablelists.org To: biofuel@sustainablelists.org Subject: [Biofuel] tirating a virgin oil Date: Sun, 20 Aug 2006 19:31:26 +0200 Hi, Recently I've came through problems with testing a cheap virgin oil in my test processor which every time ended up with incomplete reactions (emulsion problems). I did make the process longer (2 hours) and at higher temperature (60-63 degC) - still nothing, though by product separation is very nice. Today, I tried to titrate the oil and - to my surprise - it took 0.925ml of KOH solution. This was my first experience with titration, so I can also tell that the phenolophtalein solution turned pale (but noticable) magenta for about 15 secs (as described at JtF) after 0.925ml. After adding 1.05ml the colour got more intensive for longer time. My main question is - is it normal in case of cheap oils ? I suppose they contain (as other oils) some amount of FFAs, but so much ? Additional matter is whether I got titration right. I mean, interpreting the colours. I'm running out of ideas what could be wrong in the process, so any help is appreciated. -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org
Re: [Biofuel] tirating a virgin oil
Jan; Thank you very much for that tidbit of information. 0.5% is that by weight or volume? I use heat and vacuum to dry my oil prior to the process and I regulary can remove 1% v/v water from oil that looks very clear and has no liquid water at the bottom. On occasion I have been impatient with the vacuum drying and have run a batch with 'some' water content of which I have no idea but not had a problem. This is the first I have seen a definitive number offered for the limit on water content. Thank you. Joe Jan Warnqvist wrote: Hello Emre, Rafal et al. I have to say that I partially disagree with some of your statements. The limit of FFA for a flawless trans-esterification is drawn at 5mg KOH/g of oil. Any value above will demand pre-treatment of the oil. It is always important to check the water content, which should be below 0,5%. Try to get hold of a water-in-oil test kit for quick determination. If we are talking about the EN standard, it is always necessary to process the oil/catalyst/methanol mix for 90 minutes to obtain the right values for tri- di- and monoglycerides. And - this assumes that you have correct stochiometric conditions and no methanol losses during processing. As for the phophatides and the chlorophyll compounds, my experience is that these are not very important for the processing result, unless the values of these are extremely high (thousands of ppms). If so, the oil is usually very dark. Totally refined oil, on the other hand, may have preservatives added, and some of these will eat catalyst. So, good oil quality is a tricky thing. Best of luck to you ! Jan Warnqvist AGERATEC AB + 46 554 201 89 +46 70 499 38 45 - Original Message - From: "EMRE ELMAS" [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Sunday, August 20, 2006 10:15 PM Subject: Re: [Biofuel] tirating a virgin oil Dear Rafal, First of all, as long as you use cheap oil you should always be prepared to deal with much more FFA and water than it should normally contain. I think your emulsion problem occurs as a result of highly contained water. If that is the problem you should first dry the oil then process the reaction. Also if you use crude oil you should be very careful about the chemicals, such as lesitine, in the oil. So always try to use degummed oil, if you have to process crude oil. Another thing is, as you probably know, approximately 95 - 97 % of the reaction is completed in the first 35 minutes, so you do not have to wait for 2 hours. Also the alcohol boils at 65 C and the closer you get to that point, the more alcohol you will lose at the time you need it the most for the reaction. This prevents you to complete the reaction 100 %. As I mentioned above if you just watch the content of water and the other impurities in the oil you will be fine. Hopefully the information works for you. I am looking forward to hear from you soon. Best wishes, Emre ELMAS Mobile: +90 533 517 72 45 From: Rafal Szczesniak [EMAIL PROTECTED] Reply-To: biofuel@sustainablelists.org To: biofuel@sustainablelists.org Subject: [Biofuel] tirating a virgin oil Date: Sun, 20 Aug 2006 19:31:26 +0200 Hi, Recently I've came through problems with testing a cheap virgin oil in my test processor which every time ended up with incomplete reactions (emulsion problems). I did make the process longer (2 hours) and at higher temperature (60-63 degC) - still nothing, though by product separation is very nice. Today, I tried to titrate the oil and - to my surprise - it took 0.925ml of KOH solution. This was my first experience with titration, so I can also tell that the phenolophtalein solution turned pale (but noticable) magenta for about 15 secs (as described at JtF) after 0.925ml. After adding 1.05ml the colour got more intensive for longer time. My main question is - is it normal in case of cheap oils ? I suppose they contain (as other oils) some amount of FFAs, but so much ? Additional matter is whether I got titration right. I mean, interpreting the colours. I'm running out of ideas what could be wrong in the process, so any help is appreciated. -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ _ Don't just search. F
Re: [Biofuel] tirating a virgin oil
On Mon, Aug 21, 2006 at 10:08:58AM -0400, Thomas Kelly wrote: Rafal, 1 - 2L test batches w. virgin oil . Good 99% pure KOH V. Good (If you are concerned about the purity and have NaOH of known purity you can test the KOH) I know that. However, KOH that I've bought doesn't look perfectly fresh ie. it is not completely translucent, as my NaOH was a couple of months ago. Now, I have both of them slightly calcinated which shows up as a trace of dust (really, just a little bit) on the bottom of a bottle I use to mix the methoxide solution. Temp and agitation also sound good. If there is water in the methanol you will make more soap (emulsion) and there will be less methanol --- incomplete reaction (emulsion). No, the methanol is also very pure - the same supplier. I started with pure and a bit expensive chemicals, to gain more experience and avoid troubles that might be caused by urity. As I understand it, you have done test batches w virgin oil and have gotten unsatisfactory results emulsions upon washing. You are concerned about incomplete reactions. That's right. Question #1: Are you careful to exclude the glycerine byproduct from the wash? Last time I settled the mixture of ester and glycerine byproduct for 24 hours and got nice separation. I carefully removed glycerine from the bottom (similar construction to the test processor on JtF pages) _and_ I settled the ester with just a bit of byproduct on the bottom (difficult to remove completely) for the next 12 hours. Then I syphoned off a 200 ml sample for test using elastic pipe, from the middle of the container. Nice, clean and pale yellow product. My only concern is that it's not transparent, but rather cloudy - likely due to incomplete reaction. Question #2: The oil titrated at 0.925 ml of .99KOH.. This is significant. Have you run a batch with an additional .9 - 1.0 g KOH/L you got from titration? Not yet - that's why I'm asking for your opinion. After the mails I've received I'm going to try it. I tried it once, with NaOH, but I didn't add such a small amount (divided by 1.4), but rather 20% more. I was afraid of the lye calcination, so I tried to add more, according to what I read. That was probably too much - no luck and washing problems. 3.5g 100%NaOH/L of oil = 4.9 g 100%KOH/L of oil Of course, I realise that. Add 0.9 - 1.0 g of the KOH (from titration) you would be using 5.8 - 5.9 g of KOH/L of oil. This additional .9 -1.0 g represents an increase of 18 - 20% over the amount used for virgin oil w/o FFAs. When you consider that your KOH may be less than 99% pure, the amount needed would be even higher. This could very well be the cause of the incomplete reaction. Treat the virgin oil as if it was WVO. Include your titration results in the amount of KOH to be added and run a batch exactly as you have before. Let us know how it worked out and we'll proceed from there. Surely I will. Of course you could go out and buy some high quality veg oil that titrates zero, but then we would not get the answer to the puzzle. Exactly. Besides, led by curiousity, I tried to titrate a better oil I had. It was also pure rapeseed oil, just the quality was better. Titration result was .750ml or so. I wonder, what would be the result when a really fine quality oil was tested (sunflower perhaps)... -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
On Mon, Aug 21, 2006 at 09:57:30AM +0200, Tonom?r Andr?s wrote: Hi Rafal, If it is virgin oil from the supermarket, you should not worry about water. Yes, that's exactly what it is. Cheap brand made for a supermarket by a known oil producer (n-th pressing of residues after they make their own good oil, probably...). I had the same problem in my early batches, and I think it is the lye. do some additional test batches with more and more lye. This eay you have an idea and a feel for the process. ok, I will. According to titration results. What you should look for is a perfect wash test. Increase the lye in the batch until you can shake the hell out of it in the wash test and still get perfect separation within minutes. This is what I would be doing. Thanks for your suggestion. -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
I have found if you use a 2 liter bottle for the test batch and put a sipping nipple as found on sports bottles turn the test batch bottle upside down let it settle for the 12 to 24 hours the glycerin will drain out into a jar very well. I don't stop at thee end of the glycerin. I get a few ounces of bio then stop. I have never had a failed test batch this way at least not for glycerin being in the mix. Good luck Derick -Original Message- From: [EMAIL PROTECTED] [mailto:[EMAIL PROTECTED] On Behalf Of Rafal Szczesniak Sent: Monday, August 21, 2006 12:22 PM To: biofuel@sustainablelists.org Subject: Re: [Biofuel] tirating a virgin oil On Mon, Aug 21, 2006 at 10:08:58AM -0400, Thomas Kelly wrote: Rafal, 1 - 2L test batches w. virgin oil . Good 99% pure KOH V. Good (If you are concerned about the purity and have NaOH of known purity you can test the KOH) I know that. However, KOH that I've bought doesn't look perfectly fresh ie. it is not completely translucent, as my NaOH was a couple of months ago. Now, I have both of them slightly calcinated which shows up as a trace of dust (really, just a little bit) on the bottom of a bottle I use to mix the methoxide solution. Temp and agitation also sound good. If there is water in the methanol you will make more soap (emulsion) and there will be less methanol --- incomplete reaction (emulsion). No, the methanol is also very pure - the same supplier. I started with pure and a bit expensive chemicals, to gain more experience and avoid troubles that might be caused by urity. As I understand it, you have done test batches w virgin oil and have gotten unsatisfactory results emulsions upon washing. You are concerned about incomplete reactions. That's right. Question #1: Are you careful to exclude the glycerine byproduct from the wash? Last time I settled the mixture of ester and glycerine byproduct for 24 hours and got nice separation. I carefully removed glycerine from the bottom (similar construction to the test processor on JtF pages) _and_ I settled the ester with just a bit of byproduct on the bottom (difficult to remove completely) for the next 12 hours. Then I syphoned off a 200 ml sample for test using elastic pipe, from the middle of the container. Nice, clean and pale yellow product. My only concern is that it's not transparent, but rather cloudy - likely due to incomplete reaction. Question #2: The oil titrated at 0.925 ml of .99KOH.. This is significant. Have you run a batch with an additional .9 - 1.0 g KOH/L you got from titration? Not yet - that's why I'm asking for your opinion. After the mails I've received I'm going to try it. I tried it once, with NaOH, but I didn't add such a small amount (divided by 1.4), but rather 20% more. I was afraid of the lye calcination, so I tried to add more, according to what I read. That was probably too much - no luck and washing problems. 3.5g 100%NaOH/L of oil = 4.9 g 100%KOH/L of oil Of course, I realise that. Add 0.9 - 1.0 g of the KOH (from titration) you would be using 5.8 - 5.9 g of KOH/L of oil. This additional .9 -1.0 g represents an increase of 18 - 20% over the amount used for virgin oil w/o FFAs. When you consider that your KOH may be less than 99% pure, the amount needed would be even higher. This could very well be the cause of the incomplete reaction. Treat the virgin oil as if it was WVO. Include your titration results in the amount of KOH to be added and run a batch exactly as you have before. Let us know how it worked out and we'll proceed from there. Surely I will. Of course you could go out and buy some high quality veg oil that titrates zero, but then we would not get the answer to the puzzle. Exactly. Besides, led by curiousity, I tried to titrate a better oil I had. It was also pure rapeseed oil, just the quality was better. Titration result was .750ml or so. I wonder, what would be the result when a really fine quality oil was tested (sunflower perhaps)... -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html
[Biofuel] tirating a virgin oil
Hi, Recently I've came through problems with testing a cheap virgin oil in my test processor which every time ended up with incomplete reactions (emulsion problems). I did make the process longer (2 hours) and at higher temperature (60-63 degC) - still nothing, though by product separation is very nice. Today, I tried to titrate the oil and - to my surprise - it took 0.925ml of KOH solution. This was my first experience with titration, so I can also tell that the phenolophtalein solution turned pale (but noticable) magenta for about 15 secs (as described at JtF) after 0.925ml. After adding 1.05ml the colour got more intensive for longer time. My main question is - is it normal in case of cheap oils ? I suppose they contain (as other oils) some amount of FFAs, but so much ? Additional matter is whether I got titration right. I mean, interpreting the colours. I'm running out of ideas what could be wrong in the process, so any help is appreciated. -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
Rafal, I assume you are doing 1L test batches? Correct me if I'm wrong. Do you know the purity of the KOH you are using? I have heard of virgin oil containing some FFA. I have no experience with such oil. Your interpretation of the titration color sounds fine to me. The difference between .925 g KOH and 1.05 g KOH represents a 1 - 2 % difference in the amount of caustic/L of oil and would be insignificant compared to the approximately 15% difference in caustic needed for oil that titrates .925ml KOH and virgin oil that titrates to 0ml. Don't despair. Overcoming obstacles early on is part of the learning process. It is why one should start with small (1L) test batches. Best of luck, Tom - Original Message - From: Rafal Szczesniak [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Sunday, August 20, 2006 1:31 PM Subject: [Biofuel] tirating a virgin oil Hi, Recently I've came through problems with testing a cheap virgin oil in my test processor which every time ended up with incomplete reactions (emulsion problems). I did make the process longer (2 hours) and at higher temperature (60-63 degC) - still nothing, though by product separation is very nice. Today, I tried to titrate the oil and - to my surprise - it took 0.925ml of KOH solution. This was my first experience with titration, so I can also tell that the phenolophtalein solution turned pale (but noticable) magenta for about 15 secs (as described at JtF) after 0.925ml. After adding 1.05ml the colour got more intensive for longer time. My main question is - is it normal in case of cheap oils ? I suppose they contain (as other oils) some amount of FFAs, but so much ? Additional matter is whether I got titration right. I mean, interpreting the colours. I'm running out of ideas what could be wrong in the process, so any help is appreciated. -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
On Sun, Aug 20, 2006 at 06:29:51PM -0400, Thomas Kelly wrote: Rafal, I assume you are doing 1L test batches? Correct me if I'm wrong. Yes. Actually these are 1 or 2l test batches. For agitation I use a small water pump originally designed for larger aquaria and also recently used in water cooling systems for PCs. Manufacturer says it's capacity is 700 liters per hour. Even considering higher viscosity of oil it should be enough for 5l testing container. Do you think it is ? I can provide some pictures if it helps (I've done a bit of documentation). Do you know the purity of the KOH you are using? Yes, it's 99% pure from chemical supplier, though I've noticed it's a little bit calcinated (some flakes are too white, in my opinion). I have also tried NaOH (same purity) before with the same result. I have heard of virgin oil containing some FFA. I have no experience with such oil. It's probably normal, as it sounds impossible to make fresh oil with absolutely no FFAs. The question is - what amount is 'normal' and what is definately not ? -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] tirating a virgin oil
Dear Rafal, First of all, as long as you use cheap oil you should always be prepared to deal with much more FFA and water than it should normally contain. I think your emulsion problem occurs as a result of highly contained water. If that is the problem you should first dry the oil then process the reaction. Also if you use crude oil you should be very careful about the chemicals, such as lesitine, in the oil. So always try to use degummed oil, if you have to process crude oil. Another thing is, as you probably know, approximately 95 - 97 % of the reaction is completed in the first 35 minutes, so you do not have to wait for 2 hours. Also the alcohol boils at 65 C and the closer you get to that point, the more alcohol you will lose at the time you need it the most for the reaction. This prevents you to complete the reaction 100 %. As I mentioned above if you just watch the content of water and the other impurities in the oil you will be fine. Hopefully the information works for you. I am looking forward to hear from you soon. Best wishes, Emre ELMAS Mobile: +90 533 517 72 45 From: Rafal Szczesniak [EMAIL PROTECTED] Reply-To: biofuel@sustainablelists.org To: biofuel@sustainablelists.org Subject: [Biofuel] tirating a virgin oil Date: Sun, 20 Aug 2006 19:31:26 +0200 Hi, Recently I've came through problems with testing a cheap virgin oil in my test processor which every time ended up with incomplete reactions (emulsion problems). I did make the process longer (2 hours) and at higher temperature (60-63 degC) - still nothing, though by product separation is very nice. Today, I tried to titrate the oil and - to my surprise - it took 0.925ml of KOH solution. This was my first experience with titration, so I can also tell that the phenolophtalein solution turned pale (but noticable) magenta for about 15 secs (as described at JtF) after 0.925ml. After adding 1.05ml the colour got more intensive for longer time. My main question is - is it normal in case of cheap oils ? I suppose they contain (as other oils) some amount of FFAs, but so much ? Additional matter is whether I got titration right. I mean, interpreting the colours. I'm running out of ideas what could be wrong in the process, so any help is appreciated. -- cheers, Rafal Szczesniak **mir[at]diament.iit.pwr.wroc.pl Samba Team member mi***[at]samba.org +-+ *BSD, GNU/Linux and Samba http://www.samba.org +-+ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/ _ Dont just search. Find. Check out the new MSN Search! http://search.msn.click-url.com/go/onm00200636ave/direct/01/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
