Ingram Research Project

Melissa Ingram (Edgewood Jr./Sr. High Student) BioDiesel Research Project Brevard Regional Science and Engineering Science Fair Winner Also at: Orlando Science Center Science Challenge March 11-12 2005 State of Florida State Science and Engineering Fair, Orange County Convention Center, Orlando, April 6-9 2005
Plan (note that "third change to the testing procedure, listed under the heading "Subsequent Experiments" is the one that produced the best resulting fuel")		Results (Complete results pending)
Title BIOdiesel - The Homemade Alternative to Diesel Fuel Purpose Can biodiesel, one of the leading alternative fuels to petroleum-diesel, be easily produced at a high quality, then blended in a solution with diesel to be used in a truck's compression-ignition engine? What are biodiesel's basic properties and how do they compare with diesel and biodiesel/diesel blends? The first purpose of this experiment is to see if making a renewable, biodegradable, and low-pollution fuel is achievable. Second is to see how the fuel compares with its more common and more polluting rival, petroleum-diesel, in cold weather properties, specific gravity, and copper strip corrosion, as well as emissions data gathered from previous researchers' results. My hope for this experiment is that I prove how easy it is for an individual to significantly reduce air, land, and water pollution while decreasing dependancy on oil from the Middle East. Hypothesis Based on my research studies thus far, I believe I can make a high-quality fuel fit for use in a diesel engine without the harmful effects associated with petroleum-diesel. Biodiesel's cold weather properties are not as good as diesel's, it has a higher specific gravity, corrodes at a rate less than or roughly equal to diesel, and reduces emissions greatly, compared to diesel. Procedures Note: Before starting any experiments it is necessary to put on long sleeves and pants, closed-toe shoes, and make available/wear the "Necessary Safety Equipment" listed above. Make sure to be in an area with proper ventilation. It is also very important to keep everything DRY. Both methanol and NaOH are highly hygroscopic. Remember, sodium hydroxide, methanol, and methoxide are very dangerous chemicals and should be treated as such. Do not breathe the fumes. Do not leave dangerous chemicals exposed to air - measure out and close. A) Control Experiment 1. Collect necessary supplies and Ingredients for this experiment - 1L new soybean oil, 200mL methanol, 3.5g lye (sodium hydroxide), glass blender, electronic scale, empty yogurt container, tall glass bottle with narrow neck, graduated cylinder (mL), measuring cup(s) 2. Measure out the correct amount of oil first, using measuring cup(s). Then measure out the methanol in graduated cylinder and pour methanol only into the blender. Replace blender cap. 3. Measure out lye quickly on scale with a dry piece of yogurt container and add to blender immediately. Turn blender on 6th out of 12 speeds or the equivalent; mix until lye is completely dissolved. (Should take around 2-4 min.) This is called "methoxide." 4. Add oil to methoxide in blender; mix for 15 minutes or until foamy. Do not allow mixture to foam over blender lid. 5. Pour into glass bottle, allow to settle for 12 hours, then siphon off biodiesel, if possible. B) Subsequent Experiments 1. Repeat process described above, but change the amount of lye to 4.5g. 2. Repeat, but use 4.5g lye and heat oil to 120F in cooking pan on single burner, using thermometer to check temp., as described below. a. Heating the oil b. Measure out 1L new oil into a pan large enough to hold 1L. c. Place pan on burner, turn on to low-med. power. d. Check temp. frequently, as oil heats rather quickly and takes a comparatively longer time to cool down to 120F than it does to heat up to that temp. Note: The oil might not be exactly 120F. This is fine. As long as temp. is within 120-135F, proceed. Why? Any temp. higher than 135F presents the risk of the methanol boiling, which boils at 148F. It will evaporate before the reaction is complete and also releases highly combustible fumes, a major safety hazard. 3. Repeat, using 4.5g lye, heat oil to 120F, mix both the methoxide and methoxide &oil on lowest blender speed. 4. Repeat, using 4.5g lye, oil at 120F, mix methoxide and oil together on lowest blender speed, but mix methoxide "by hand", as described below. a. Ingredients and Materials: 200mL methanol, 4.5g lye; 1sm. Mason jar with lid. b. Measure out methanol into jar, add 1g lye. Close lid firmly and shake until dissolved. c. Add 1.5g lye, shake until dissolved. d. Add remaining 2g lye, shake until dissolved. Note: Because methanol and lye do not readily mix, this may take around 10 min. to complete. It is not ready until NO lye crystals can be seen and the methoxide is slightly cloudy. C) Quality Test 1. Measure out 200mL biodiesel, not biodiesel/glycerine mix into lrg Mason jar. Add enough water to make 400mL. 2. Shake container for 10 sec., then allow to sit. 3. Results: A respectable quality biodiesel will separate from water in 30 min. or less to form only two layers - clear, light-yellow biodiesel and milky water. D) The Wash 1. Separate biodiesel from glycerine; place in a lrg. Container (like a 2 or 5 gal. fish bowl). 2. Add 50 % water (500mL). 3. Plug tubing and bubble bar into aerator; attach bar to bottom/side inside tank (as long as in stays submerged it's fine); plug aerator into electric outlet. 4. Let it be for 12 hrs., unplug from outlet, remove water. Add new water, let run again for twelve hours; repeat. 5. Siphon off biodiesel; run through fine mesh (like cheesecloth). 6. Repeat quality test: now good biodiesel should separate from water in no more than 15 min. It is now ready to be used with confidence. E) Disposal 1. If biodiesel is not of a high quality, it is okay to burn in small amounts. 2. Glycerine makes a very good soap/degreaser. A. Heat glycerine to 155 degreesF (65.5C) to get rid of excess methanol. B. Cut with water and/or if soft enough already, pour into empty soap dispenser and use as a soap/degreaser. F) Testing cold weather properties 1. Materials and Ingredients: pan for ice bath, 500mL capacity graduated beaker, 200mL washed biodiesel, thermometer. 2. Put on gloves, apron, goggles; make safety equipment available. 3. Measure out biodiesel into beaker; fill ice bath; place beaker in pan. 4. Monitor temperature periodically. When fuel starts to cloud, take temp. and record as "cloud point." 5. Continue monitoring sample; every 3degrees C, tip jar lightly to one side. When sample ceases movement, record temp. as "pour point." G) Measuring specific gravity 1. Ingredients and Materials: 300mL washed biodiesel, beaker, hydrometer. 2. Place biodiesel sample in beaker; fill to near the top of the beaker. 3. Place hydrometer in sample; take measurement at the meniscus. Record. H) Testing Copper Strip Corrosion 1. Ingredients and Materials: 300mL biodiesel; polished copper strips, beaker, hot plate 2. Fill beaker with fuel sample; put on hot plate; bring temp. to 50degrees C and maintain temp. 3. Add copper strip; allow to sit on hot plate for 3hours. 4. Remove strip with forceps; wash lightly in solvent.		Results In the first experiment, I used a 5:1 ratio of soybean oil to methanol. (That ratio remained constant throughout all experiments.) With the recommended amount of lye (catalyst) when using new oil (.35% amount vegetable oil used) and a room temperature reaction on the 6th of 12 blender speeds, the biodiesel resulting was filled with contaminants and soap residue. It was a golden color, translucent, with dark brown, low viscosity glycerine. The glycerine took over a week to harden, and even then it was not a high quality. A quality test revealed just how foul the batch was - instead of taking 30 minutes to separate from water, the biodiesel took a full 3 days to separate, and it separated into 3 layers. From bottom to top they were 1) thick dark yellow, 2) opaque white soap, and 3) white/light yellow watery substance. For the second experiment, 5:1 ratio remained the same, as well as the temperature of reaction, and the blender speed. I changed the amount of catalyst to .45% in order to speed up the reaction and make it more complete. The biodiesel resulting was filled with contaminants and soap residue, golden in color, translucent, with dark brown, low viscosity glycerine. The glycerine took a week to harden, and the biodiesel separated from water in 3 days, not 30 minutes. It continued to separate throughout the course of the experiment, separating into 3 layers (From bottom to top they were 1. thick dark yellow, 2. opaque white soap, and 3. white/light yellow watery substance.) Anytime soap is formed, something in the process went awry. This is one the main reasons why I was able to determine the poor quality of the fuel. The 5:1 ratio remained the same in the 3rd experiment, .45% catalyst was used, the 6th out of 12 blender speeds was used for all mixing, but the reaction took place at 120F, not room temperature. During the mixing the temperature rose to a sweltering 140F. The biodiesel resulting was filled with contaminants and soap residue, golden in color, translucent, with dark brown, low viscosity glycerine that took nearly three days to harden. I did not perform a quality test on this batch because it was so identical to the first 2 batches. This was very unscientific, and I regret it now, but I still think nothing notable would have resulted from the test. In the 4th experiment, the 5:1 ratio, .45% catalyst, and reaction temperature of 120F all remained constant. Instead of mixing the methoxide and the methoxide/oil on the 6th out of 12 blender speeds, I mixed both on the lowest blender speed. The temperature decreased 3degrees to 117F during the mixing. The biodiesel's quality was remarkably better than that of the first 3 batches. The biodiesel was clear and light, as well as was the glycerine, which took 2 days to harden. It separated into only 2 distinct layers during the quality test, clear, light biodiesel on top and cloudy water below. The biodiesel in the quality test was almost identical to the biodiesel in the container - a great sign. All of my research revealed that a batch that separates like the 4th did is a very high quality fuel. Although it did take 2 days for the glycerine to harden, and also over a week for the clear layer of biodiesel to form on top of the white water in the quality test, so I knew my testing wasn't complete and I needed to further improve my process. In the 5th experiment the 5:1 ratio, .45% catalyst, temperature at 120F, and methoxide/oil was mixed on the lowest blender speed, but the methoxide alone (methanol and lye) was mixed by hand in a Mason jar. The temperature increased 5 degrees to 125F during the mixing. The glycerine formed in 2 days and continued to harden for a week, when it was extremely hard and looked very good. The 2 layers in the quality test separated into only 2 layers, like the 4th batch, but the layers looked extremely different. There was dark yellow biodiesel on top and a different shade of white water on the bottom. It separated in less than 9 hours into these perfect 2 layers, the fastest yet.

Melissa Ingram (Edgewood Jr./Sr. High Student)
BioDiesel Research Project
Brevard Regional Science and Engineering Science Fair Winner
Also at:
Orlando Science Center Science Challenge March 11-12 2005
State of Florida State Science and Engineering Fair, Orange County Convention Center, Orlando, April 6-9 2005

Plan
(note that "third change to the testing procedure, listed under the heading "Subsequent Experiments" is the one that produced the best resulting fuel")

Results
(Complete results pending)

Title
BIOdiesel - The Homemade Alternative to Diesel Fuel
Purpose
Can biodiesel, one of the leading alternative fuels to petroleum-diesel, be easily produced at a high quality, then blended in a solution with diesel to be used in a truck's compression-ignition engine? What are biodiesel's basic properties and how do they compare with diesel and biodiesel/diesel blends?
The first purpose of this experiment is to see if making a renewable, biodegradable, and low-pollution fuel is achievable. Second is to see how the fuel compares with its more common and more polluting rival, petroleum-diesel, in cold weather properties, specific gravity, and copper strip corrosion, as well as emissions data gathered from previous researchers' results.
My hope for this experiment is that I prove how easy it is for an individual to significantly reduce air, land, and water pollution while decreasing dependancy on oil from the Middle East.
Hypothesis
Based on my research studies thus far, I believe I can make a high-quality fuel fit for use in a diesel engine without the harmful effects associated with petroleum-diesel. Biodiesel's cold weather properties are not as good as diesel's, it has a higher specific gravity, corrodes at a rate less than or roughly equal to diesel, and reduces emissions greatly, compared to diesel.
Procedures
*Note: Before starting any experiments it is necessary to put on long sleeves and pants, closed-toe shoes, and make available/wear the "Necessary Safety Equipment" listed above. Make sure to be in an area with proper ventilation. It is also very important to keep everything DRY. Both methanol and NaOH are highly hygroscopic. Remember, sodium hydroxide, methanol, and methoxide are very dangerous chemicals and should be treated as such. Do not breathe the fumes. Do not leave dangerous chemicals exposed to air - measure out and close.
A) Control Experiment
1. Collect necessary supplies and Ingredients for this experiment - 1L new soybean oil, 200mL methanol, 3.5g lye (sodium hydroxide), glass blender, electronic scale, empty yogurt container, tall glass bottle with narrow neck, graduated cylinder (mL), measuring cup(s)
2. Measure out the correct amount of oil first, using measuring cup(s). Then measure out the methanol in graduated cylinder and pour methanol only into the blender. Replace blender cap.
3. Measure out lye quickly on scale with a dry piece of yogurt container and add to blender immediately. Turn blender on 6th out of 12 speeds or the equivalent; mix until lye is completely dissolved. (Should take around 2-4 min.) This is called "methoxide."
4. Add oil to methoxide in blender; mix for 15 minutes or until foamy. Do not allow mixture to foam over blender lid.
5. Pour into glass bottle, allow to settle for 12 hours, then siphon off biodiesel, if possible.
B) Subsequent Experiments
1. Repeat process described above, but change the amount of lye to 4.5g.
2. Repeat, but use 4.5g lye and heat oil to 120F in cooking pan on single burner, using thermometer to check temp., as described below.
a. Heating the oil
b. Measure out 1L new oil into a pan large enough to hold 1L.
c. Place pan on burner, turn on to low-med. power.
d. Check temp. frequently, as oil heats rather quickly and takes a comparatively longer time to cool down to 120F than it does to heat up to that temp.
*Note: The oil might not be exactly 120F. This is fine. As long as temp. is within 120-135F, proceed. Why? Any temp. higher than 135F presents the risk of the methanol boiling, which boils at 148F. It will evaporate before the reaction is complete and also releases highly combustible fumes, a major safety hazard.
3. Repeat, using 4.5g lye, heat oil to 120F, mix both the methoxide and methoxide &oil on lowest blender speed.
4. Repeat, using 4.5g lye, oil at 120F, mix methoxide and oil together on lowest blender speed, but mix methoxide "by hand", as described below.
a. Ingredients and Materials: 200mL methanol, 4.5g lye; 1sm. Mason jar with lid.
b. Measure out methanol into jar, add 1g lye. Close lid firmly and shake until dissolved.
c. Add 1.5g lye, shake until dissolved.
d. Add remaining 2g lye, shake until dissolved.**
**Note: Because methanol and lye do not readily mix, this may take around 10 min. to complete. It is not ready until NO lye crystals can be seen and the methoxide is slightly cloudy.
C) Quality Test
1. Measure out 200mL biodiesel, not biodiesel/glycerine mix into lrg Mason jar. Add enough water to make 400mL.
2. Shake container for 10 sec., then allow to sit.
3. Results: A respectable quality biodiesel will separate from water in 30 min. or less to form only two layers - clear, light-yellow biodiesel and milky water.
D) The Wash
1. Separate biodiesel from glycerine; place in a lrg. Container (like a 2 or 5 gal. fish bowl).
2. Add 50 % water (500mL).
3. Plug tubing and bubble bar into aerator; attach bar to bottom/side inside tank (as long as in stays submerged it's fine); plug aerator into electric outlet.
4. Let it be for 12 hrs., unplug from outlet, remove water. Add new water, let run again for twelve hours; repeat.
5. Siphon off biodiesel; run through fine mesh (like cheesecloth).
6. Repeat quality test: now good biodiesel should separate from water in no more than 15 min.
It is now ready to be used with confidence.
E) Disposal
1. If biodiesel is not of a high quality, it is okay to burn in small amounts.
2. Glycerine makes a very good soap/degreaser.
A. Heat glycerine to 155 degreesF (65.5C) to get rid of excess methanol.
B. Cut with water and/or if soft enough already, pour into empty soap dispenser and use as a soap/degreaser.
F) Testing cold weather properties
1. Materials and Ingredients: pan for ice bath, 500mL capacity graduated beaker, 200mL washed biodiesel, thermometer.
2. Put on gloves, apron, goggles; make safety equipment available.
3. Measure out biodiesel into beaker; fill ice bath; place beaker in pan.
4. Monitor temperature periodically. When fuel starts to cloud, take temp. and record as "cloud point."
5. Continue monitoring sample; every 3degrees C, tip jar lightly to one side. When sample ceases movement, record temp. as "pour point."
G) Measuring specific gravity
1. Ingredients and Materials: 300mL washed biodiesel, beaker, hydrometer.
2. Place biodiesel sample in beaker; fill to near the top of the beaker.
3. Place hydrometer in sample; take measurement at the meniscus. Record.
H) Testing Copper Strip Corrosion
1. Ingredients and Materials: 300mL biodiesel; polished copper strips, beaker, hot plate
2. Fill beaker with fuel sample; put on hot plate; bring temp. to 50degrees C and maintain temp.
3. Add copper strip; allow to sit on hot plate for 3hours.
4. Remove strip with forceps; wash lightly in solvent.

Results
In the first experiment, I used a 5:1 ratio of soybean oil to methanol. (That ratio remained constant throughout all experiments.) With the recommended amount of lye (catalyst) when using new oil (.35% amount vegetable oil used) and a room temperature reaction on the 6th of 12 blender speeds, the biodiesel resulting was filled with contaminants and soap residue. It was a golden color, translucent, with dark brown, low viscosity glycerine. The glycerine took over a week to harden, and even then it was not a high quality. A quality test revealed just how foul the batch was - instead of taking 30 minutes to separate from water, the biodiesel took a full 3 days to separate, and it separated into 3 layers. From bottom to top they were 1) thick dark yellow, 2) opaque white soap, and 3) white/light yellow watery substance.

For the second experiment, 5:1 ratio remained the same, as well as the temperature of reaction, and the blender speed. I changed the amount of catalyst to .45% in order to speed up the reaction and make it more complete. The biodiesel resulting was filled with contaminants and soap residue, golden in color, translucent, with dark brown, low viscosity glycerine. The glycerine took a week to harden, and the biodiesel separated from water in 3 days, not 30 minutes. It continued to separate throughout the course of the experiment, separating into 3 layers (From bottom to top they were 1. thick dark yellow, 2. opaque white soap, and 3. white/light yellow watery substance.) Anytime soap is formed, something in the process went awry. This is one the main reasons why I was able to determine the poor quality of the fuel.

The 5:1 ratio remained the same in the 3rd experiment, .45% catalyst was used, the 6th out of 12 blender speeds was used for all mixing, but the reaction took place at 120F, not room temperature. During the mixing the temperature rose to a sweltering 140F. The biodiesel resulting was filled with contaminants and soap residue, golden in color, translucent, with dark brown, low viscosity glycerine that took nearly three days to harden. I did not perform a quality test on this batch because it was so identical to the first 2 batches. This was very unscientific, and I regret it now, but I still think nothing notable would have resulted from the test.

In the 4th experiment, the 5:1 ratio, .45% catalyst, and reaction temperature of 120F all remained constant. Instead of mixing the methoxide and the methoxide/oil on the 6th out of 12 blender speeds, I mixed both on the lowest blender speed. The temperature decreased 3degrees to 117F during the mixing. The biodiesel's quality was remarkably better than that of the first 3 batches. The biodiesel was clear and light, as well as was the glycerine, which took 2 days to harden. It separated into only 2 distinct layers during the quality test, clear, light biodiesel on top and cloudy water below. The biodiesel in the quality test was almost identical to the biodiesel in the container - a great sign. All of my research revealed that a batch that separates like the 4th did is a very high quality fuel. Although it did take 2 days for the glycerine to harden, and also over a week for the clear layer of biodiesel to form on top of the white water in the quality test, so I knew my testing wasn't complete and I needed to further improve my process.

In the 5th experiment the 5:1 ratio, .45% catalyst, temperature at 120F, and methoxide/oil was mixed on the lowest blender speed, but the methoxide alone (methanol and lye) was mixed by hand in a Mason jar. The temperature increased 5 degrees to 125F during the mixing. The glycerine formed in 2 days and continued to harden for a week, when it was extremely hard and looked very good. The 2 layers in the quality test separated into only 2 layers, like the 4th batch, but the layers looked extremely different. There was dark yellow biodiesel on top and a different shade of white water on the bottom. It separated in less than 9 hours into these perfect 2 layers, the fastest yet.