The use of plant oil as fuel may seem insignificant today.

But such products can in time become just as important as kerosene and these coal-tar-products of today...Rudolf Diesel, 1912.

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Making biodiesel safely
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Making Biodiesel using Ethanol

It is essential that you obtain plenty of experience making biodiesel with methanol before trying to use ethanol. Making biodiesel using ethanol as one half of the reactants is more difficult than using methanol. The main reasons for this are:

Obtaining pure ethanol with less that 0.5% water is difficult More alcohol is required when using ethanol The vegetable oil needs heating to a higher temperature (120C) The reaction can be sensitive to water Potassium hydroxide works best with ethanol but can be hard to find Separation is more difficult Titrating the oil for FFAs (free fatty acids) is required when using ethanol

Again making a 1 litre test batch is a good place to start. To make 1 litre of biodiesel from SVO you will need: 1. 1 litre of unused vegetable oil; 2. 300ml of ethanol (99.5% pure); 3. 10g of potassium hydroxide (85% or higher); 4. Glass mixing container with tight fitting lid; 5. 2 litre plastic bottle; 6. 2 or 3 funnels; 7. Thermometer; 8. Scales accurate to 0.1g or less. And for the titration test: 9. Phenolphthalein or ph paper (to test for acidity - don't use phenol red indicator); 10. Bottle of distilled water (see note); 11. 1 litre bottle (for tester solution); 12. Isopropyl alcohol; 13. 3 oral syringes graduated in ml or eyedroppers; 14. Several small glass jars or beakers; 15. Stainless steel stirrers/spoons.
Water can contain microscopic contaminants along with dissolved minerals like calcium and iron. Boiling water until it changes to steam is one way to remove these, a process known as distillation. When the steam cools and condenses into liquid again, a more purified water is formed called distilled water. Ideally distilled water should simply be hydrogen and oxygen molecules with a PH level of 7 with no additional contaminants.

Sourcing the Ingredients

Vegetable oil is readily available in the supermarkets, but what about ethanol and potassium hydroxide? If you're using ethanol for environmental reasons because it is fossil-free, be aware that this isn't always the case. One way to make sure is to ensure the ethanol is synthetic rather than fermented. When using ethanol it is not wise to use sodium hydroxide because it takes too long to mix with ethanol. Potasssium hydroxide mixes much better, and with either catalyst more is required when using ethanol - 7g of

sodium hydroxide per litre of oil, and 10g of potassium hydroxide per litre of oil (or more as dictated by the titration test. These are probably best sourced from online suppliers.

Step 1a: Heat the oil

The oil needs to be very dry, and any more than 0.5% water can prevent the reaction occuring. Heat the vegetable oil to 120C (248F) in a saucepan. Keep it there until the heat can be removed and any bubbling stops almost immediately. Leave it to settle for half a day or so and take oil from the top.

Step 1b: Pre-heat the oil

Heat the oil again to 60C as (140F) as this this will make for easier mixing. Although vegetable oil has a relatively high flash point, never leave heating oil unnatended and always keep a thermometer in the pan.

Step 2: Titration test

Dissolve 1 gram of potassium hydroxide into 1 litre of distilled water to make a 'tester solution' (this can be stored for future tests). For more accuracy, dissolve 3 gram into 3 litres.

Step 2a: Blank titration test on the isopropyl alcohol

Alcohol can become a little acidic with age, which would affect the titration results. A blank titration test neutralises these acids so the real titration test only detects the free fatty acids in the oil, instead of those in the isopropyl alcohol. Add 10ml of isopropyl alcohol to a beaker. Add a few drops of phenolpthaleine and swirl (it will be a yellowish color). Add the tester solution drop by drop and keep swirling. The instant it turns purple, the acids have been neutralised so stop. If only 5 to 10 drops of tester solution were needed then it's not very acidic and this test can be omitted for the next few titrations. Otherwise a blank titration is required every time this particular alcohol is used.

Step 2b: The Titration test

Measure 1ml of oil into a jar or beaker with about 10ml of isopropyl alcohol using different syringes - note the amount of oil is crucial but not the isopropyl (the

isopropyl/phenothalein mixture from the blank titration can be used here). If a blank titration hasn't been performed add roughly 5 drops of phenolpthaleine. Swirl the jar to dissolve the contents, which will be a murky yellow color. Slowly add the tester solution drop by drop while swirling the beaker until the contents turn a pink color that lasts for 30 seconds of swirling (it will start to change to pink but will keep reverting back to yellow initially). Once it's uniformly pink and stays that way for at least 30 seconds, stop adding the tester solution and count how many mililitres have been added. Alternatively, with an eyedropper, drop the tester solution into the oil mixture 1ml at a time. After each drop check the ph level of the oil mixture with the ph paper. An eventual rise in the ph level will occur. Continue to add the tester solution, one drop at a time, until it reaches a ph of 8-9. It's worth repeating the titration test to try to obtain the same result more than once, as it is easy to make mistakes when measuring such small quantities of liquids (the liquids can be thrown down the drain too as they are fairly benign).

Step 3: Calculation
Each 1ml of tester solution added means 1 extra gram of potassium hydroxide will need to be added when making the 1 litre batch of biodiesel (to eliminate the free fatty acids in the oil). If the oil required more than 5ml potassium hydroxide then don't use it until more experience is gained. Decent restaurant oil will require about 3ml of tester solution, and really bad fast food grease can take 10ml or more (which is completely unusable with sodium hydroxide as the catalyst). Note that the titration should be done using the same catalyst intended for use in making the biodiesel.

Working With Batches Larger Than 1 Litre

Calculating materials for larger batches of biodiesel is rather straightforward. Total grams of potassium hydroxide required = number of litres of oil x (7 grams + titration results) For a 90 litre batch, for example, if the titration test results were 2ml, then 2 extra grams is required for each litre of oil. Therefore:

90 litres oil x (7g potassium hydroxide + extra 2g) : 90 x 9 = 180g potassium hydroxide is needed.

Step 4: Making the potassium ethoxide (caution required)

Using a funnel, pour 300ml of ethanol into the glass container. Ethanol absorbs water from the atmosphere so do it quickly and replace the ethanol container lid tightly. Also be quick in measuring out the potassium hydroxide because it too absorbs water, which would interfere with the biodiesel reaction. With a second dry funnel, drop the 7g of potassium hydroxide into the ethanol, replace the lid immediately and shake or swirl the mixture for about 10 minutes until all of the potassium hydroxide has dissolved. After it has disolved, top up to 300ml with fresh ethanol, as there may be some evaporation during mixing.

Step 5: Making the biodiesel

Using a clean funnel pour the warm oil into the plastic bottle and then add the potassium ethoxide. Replace the bottle top, screwing it down tightly, and shake vigorously for 30 seconds. For best results shake the mixture for 5 seconds four times over the space of an hour (no appreciable pressure is generated). The mixture normally turns an orange-brown colour after a few minutes, and then to a transparent brown before becoming orange-brown again when the glycerol forms. The mixture can then be left to settle.

Step 6: Settling and Separation

Settling can be difficult, taking between 3 to 4 hours or overnight. When the glycerine has settled at the bottom with biodiesel appearing at the top - seperation has occured. The glycerine layer is usually about the same or slightly more than the amount of ethanol used. It is best to leave the mixture overnight to settle more fully. Slowly pour off the biodiesel to use as fuel and put the glycerine on your compost heap or use it to make soap (expose the glycerine to air and sunlight for 1 week first). If it refuses to

separate this is not biodiesel. It may be forced to separate by adding some sodium methoxide mix, or by adding a little methanol with the ethanol at the start.

Step 7: Washing
The quality of the biodiesel will be greatly improved by washing to remove more soap. Pour the 1 litre of biodiesel into another 2 litre bottle. Gently add half a litre of 40C water. Replace the top tightly and then turn the bottle end over end very gently for 30 seconds. As long as care is taken, the cloudy (soapy) water and biodiesel will separate quickly. Turn the bottle upside down and slowly release the water (which will form a layer at the bottom) using your thumb as a valve. Repeat this process 2 or 3 times, slowly increasing the level of agitation and the length of time the bottle is rotated (1 min for wash 2, and gently shake the bottle in wash 3). By washes 4 and 5 you can shake the bottle fairly vigorously although it will take considerably longer to separate. If the bottle is shaken too early an emulsion will form that will take days if not weeks to settle out. When finished the water should come out of the bottle fairly clear.

Step 8: Drying
Finally the water must be removed before using the biodiesel to prevent risk of damaging the engine. The easiest method of drying is settling. Leave the washed biodiesel, which will be very cloudy and much lighter in colour than unwashed biodiesel, for at least 2 days to settle. Water will settle to the bottom, and will also evaporate over time. This can be drained off, and once dry it will be clear and ready for use.

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