1 HOW TO MAKE A 1L TEST BATCH OF BIODIESEL FROM WASTE VEGETABLE OIL(WVO). MATERIALS REQUIRED.

2 litre of waste (used) oil with less than 1%FFA( free fatty acid) NaOH (lye/ caustic soda), at least 30g with a purity of 95% or better Methanol at least 1L with a purity of 98% or better Isopropyl alcohol (99%). Will be used as solvent for titrating oil. 0.1% NaOH solution, about 50ml EQUIPMENT REQUIRED 2- 2 litre and 2 1L HDPE (# 2 plastic) bottles in sound condition with tight fitting top and dry inside. 2- 2L PETbottles ( these will be used for washing the finished biodiesel with water) 2 0.5 inch angle valve 1 container to heat 1L of oil to 120*C to remove any water 1 Hot plate to heat oil. 1 thermometer with a range of 150*C 1 small weighing scale with a resolution of 0.1gram 1 500ml measuring cylinder 1 10ml and 2 3ml syringe 1 200ml beaker 1 Funnel. 1 small aquarium air pump and ceramic bubble stone (optional) THE TECHNIQUE: OIL PREPERATION Take one litre of wvo and heat to at least 120 deg c to remove all water. If water is present the oil will spit and pop and carry on. If there is a lot of water this could get very violent, so be careful. Once the water is gone (Oil becomes calm and there is no more spitting and popping) let the oil cool to about 60 deg C. TITRATION Take a 5ml sample of the oil and titrate it with the 0.1% NaOH solution to determine its acid value or %ffa content. The result from this titration will in ml. of 0.1% NaOH and will be used to calculate how much NaOH to use for the neutralization of the ffa to soap and the transesterification of the wvo to biodiesel. A base amount of 5g NaOH per litre of wvo (adjusted for purity) is required for the transesterification plus an amount in grams obtained from the titration for the neutralization of the ffa.

MAKING THE SODIUM METHOXIDE (NaOH dissolved in methanol) WARNING: METHOXIDE IS A POISON!!!!!!!!!! DO NOT BREATH VAPORS. WASH OFF ANY SPLASHES. MIX THE METHOXIDE IN A 1L HDPE BOTTLE. While the oil is cooling mix the calculated amount of NaOH(lye) obtained from the titration of the wvo with 250ml(25%) of methanol to form the sodium methoxide. This is more methanol than most people use (18% to 22%) but will help insure a quick reaction and a successful first batch. NaOH and Methanol do not readily mix, so a bit of time and patience is required. Don't sniff the fumes. CARTRIDGE RESPIRATORS DO NOT WORK WITH METHANOL For quickest mixing, start with the methanol at room temp (not warm). As you mix, the temp will increase substantially (the reaction is exothermic). This is normal. Make sure ALL the NaOH (lye) is dissolved. This may take 5 minutes or more. Place the NaOH/methanol into a 1L HDPE bottle, cover it tightly and shake/swirl until all the NaOH is dissolved. MAKING THE BIODIESEL. When the Oil's temp has dropped to 60 deg c or a bit less, using a funnel, pour 1 litre of the wvo into a DRY 2 litre HDPE bottle. Take the mixture of methanol/NaOH (commonly called sodium methoxide) and pour on top of the oil using the same funnel. Remove the funnel. Screw the top down TIGHT onto the bottle. Shake vigorously for about ten seconds/ 40 good shakes. Then place the bottle in a 60 deg C water bath for 5mins. Shake again for 10 seconds. Continue this process for 30 minutes. NO appreciable pressure is generated during this mixing. Now place the bottle on a table. You will observe the oil change colour from a "Light Chocolate milk to a rich, darker brown." Then, as if by magic, within 10 minutes the by-product (commonly referred to as glycerol byproduct) starts to settle out and form an increasing layer on the bottom of the bottle. Be sure to notice that you can see a very definite, slowly sinking line towards the top of the Biodiesel as the glycerol slowly settles. Within an hour, most of the glycerol byproduct will be settled out. This is referred to as separation. The biodiesel can now be separated from the glycerol and placed in a 2L PET bottle to be washed to removed most of the impurities.

3 WASHING BIODIESEL. Having just produced your first batch of biodiesel, it contains impurities such as excess methanol; NaOH; mono, di and triglycerides; soap and so on. These will have to be removed before the biodiesel can be used as fuel. A simple method of doing this is by washing with 25% to 50% water by volume. A sample of biodiesel can be washed in less than an hour using the technique described below. Be aware that Unwashed biodiesel contains soap. If you agitate your first few washes hard/violently, there is a real likelihood that the water, soap, and biodiesel will form an emulsion that may take days or weeks to separate. The three important steps in washing are GENTLY, GENTLY, GENTLY to begin with. THE TECHNIQUE: WASH # 1 Pour 1 litre biodiesel into a 2 litre PET bottle. Gently pour about 500ml tap water (preferably warm) into bottle. Screw on top with angle valve attached and closed. GENTLY rotate bottle end for end for about 30 seconds. After 30 seconds place bottle in an inverted position. If you have been GENTLE the water and Biodiesel will separate immediately. You will notice the water is somewhat milky. When the biodiesel and water have separated open the angle valve and drain the water. When water is drained, turn the bottle back up-right. You have finished wash one. WASH # 2 Pour in another 500ml water and repeat wash one, except rotate GENTLY for about 1 minute. Drain as in wash #1 You have finished wash 2. WASH # 3 Again pour in 500ml water and GENTLY shake bottle for a minute or so. When water and biodiesel separate discard water in same fashion as before. WASH # 4 Another 500ml water and a bit more agitation for about 1 min. After separation of water and biodiesel drain as above. WASH # 5 You should now be able shake fairly vigorously. Washing is finished when after shaking, water is nearly clear and with a pH of 7. Be aware that in your later washes (#4 & # 5) you should be able to shake violently. The

4 water and biodiesel will take longer to separate because the water forms tiny bubbles in the biodiesel that take time to settle out. Washed biodiesel is VERY CLOUDY, often looking like orange juice because it contains water. The water will have to be removed by drying . DRYING BIODIESEL. Place the 1L of washed biodiesel in a clean dry container and heat it to 100 deg C for a few minutes until the water has evaporated and the biodiesel is now crystal clear. It should stay clear when the heat is turned off and it is cooled. Place a sample of the cooled biodiesel in the 200ml beaker, you should be able to see through it if it is properly dried. Alternatively the biodiesel could be dried by heating it to only about 40 deg. C and bubbling air through it with an aquarium air pump and ceramic bubble stone. This is the preferred method because it reduces the risk of polymerization of the biodiesel due to extended exposure to high temp.