TESC Biodiesel Project

Operation Manual

Thank you (in no particular order) to: David Rack, Sam Stout, and Kolby Bray-Hoagland for starting the Evergreen Biodiesel Project; our faculty and staff, Melissa Barker, E.J. Zita, Dave Muehleisen, Marty Beagle and Michelle Bartlette; The Evergreen State College Clean Energy Committee for their funding; the students of Practice of Sustainable Agriculture Program and the Organic Farm caretakers, for their continuing support; Burke Anderson and Brodie Pettit for their research assistance; and Andrew York for his dedication and invaluable assistance in upgrading and expanding the Evergreen Biodiesel Project.

4th Edition: Revised May 2008 Written and compiled by: Megan P. Ellis-Treasure, John S. Kemp and Sara E. Keehfuss

The Evergreen Biodiesel Operation Manual

Table of Contents
Introduction Project History Winter and Spring 2008 Emergency Prevention Checklist Safety Procedure Emergency numbers Lab Rules Emergency Procedures Fire Chemical spills, on people, clean-up Chemical Storage and Transportation Chemical Fact Sheets Methyl Alcohol Potassium Hydroxide Operation Procedure Retrieval and Transit Materials Methods and Procedures Biodiesel Laboratory Manual Lab Equipment Master List Titration Transesterification Wash and Dry pH Test Specific Gravity Test 3/27 Test Cloud Point Test Biodiesel Production Equipment Reactor 1 Processing system Biodiesel Production and Procedure Measuring WVO Heating Potassium Methoxide Prep Transesterification Draining Glycerin Washing Drying Storage Quality Tests Maintenance Manual 5

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Pump # 1 Vinyl Tubing Leaks Manufactures Information Resources Human Resources Emergency Contacts (also see Safety Procedure Manual) Biodiesel Resources Credits and Bibliography 57

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Before you begin; familiarize yourself with the Biodiesel Safety, Chemical Safety, Operation Procedure, and Maintenance Manuals.

INTRODUCTION
Biodiesel (BD) is a liquid fuel that can be a direct replacement for petroleum-based diesel in diesel engines. The production of biodiesel using waste vegetable oil (WVO) can be explained by titration and transesterification. Titration is an initial test to measure the free fatty acid (FFA) content of the feedstock, which determines the amount of catalyst needed to create biodiesel and is a necessary test for waste oil. Transesterification is the process in which biodiesel is created by reacting alcohol, methanol or ethanol, with oil or fat in the presence of a catalyst, typically lye. After the transesterification the liquid needs to settle and separate into glycerin and biodiesel. The glycerin is drained; the biodiesel washed with water to filter out any remaining glycerin or other impurities and then allowed to dry in an open container placed in a well-ventilated area. The end results are biodiesel, glycerin, wastewater, oil and alcohol (the later two recycled or discarded depending on amounts and capabilities).
Spring 2005:

The Evergreen Biodiesel Projects mission is to build, refurbish and establish a permanent, safe, and user-friendly bio-diesel processing facility infrastructure. The infrastructure of the Biodiesel Project includes: a processing unit (located on Evergreens Organic Farm), a collection barrel (located in the basement of the CAB), and a transit barrel. By converting spent vegetable oil into useable biodiesel, the Biodiesel Project supplies Evergreens Organic Farm tractors with a renewable fuel. In addition, the Biodiesel Project aims to be a model for other schools and state institutions that aspire to produce biodiesel on-site. The Evergreen State College consumes roughly 3,500 gallons of petroleum diesel fuel annually. Of the various diesel vehicles at Evergreen, the Organic Farm possesses two four-cylinder Kubota tractors. The two tractors consume roughly 10 gallons of diesel fuel per week. On a weekly basis the cafeteria at Evergreen disposes of roughly 20 gallons of spent vegetable oil, at a cost of $50 per month. By using the spent vegetable oil, the Biodiesel Project will be able to produce roughly 500 gallons of biodiesel annually and fully suffice the Organic Farms diesel requirements. The 500 gallons of renewable fuel will displace 17 percent of the campuss annual petroleum diesel consumption. In addition, the user-friendly biodiesel infrastructure will be an excellent learning tool for faculty, students and staff in various applications. In the winter of 2004, David Rack, Sam Stout, and Kolby Bray-Hoagland researched and designed a processing unit. In the spring of 2004, David and Kolby fabricated the various components, utilizing the campus metal shop. In the summer of 2004, Kolby and Sam installed the processing unit and built a fume hood, a filtered collection barrel, and a transit barrel. In the fall of 2004, Kolby and Sam wrote a Safety Manual, Procedure

Manual, Maintenance Manual, and other related written aids for the operation and upkeep of the Biodiesel Project. Over the fall, Sam performed test batches in order to determine the quality of the spent oil. In the spring of 2005, the Biodiesel Project became fully operational. i Fall 2007: The facility was out of operation for a little over a year when John Kemp, Megan EllisTreasure and their team brought it back into production. They began safety-testing the facility in spring of 2007. The team refurbished the main reactor, tested all equipment, performed mini-test batches in the Laboratory, created a new version of the Evergreen Biodiesel Project Operation and Safety Manual, and produced several full-scale batches of biodiesel. Winter and Spring 2008: After working with the original biodiesel production equipment for over 3 quarters, Megan and John began brainstorming ways to upgrade the facility. Areas of the production system that needed improvement were numerous. After researching possible upgrades it was decided to integrate a new system into the existing biodiesel processing infrastructure. With the help of a new teammate, Andrew York, a new production system was designed and budgeted winter quarter 2008. Phase 1 of the Biodiesel Expansion Project began with a grant award from the Clean Energy Committee (CEC). The CEC awards grants to clean energy student projects, more information about the CEC and a grant application can be found here: http://www.evergreen.edu/committee/cleanenergy/home.htm. Funds granted in winter 2008 for the BEP were originally planned to cover the costs of a dedicated wash tank to reduce the time required to produce a batch of biodiesel. Additionally, the funds requested were intended to cover the costs of more minor things like safety clothing and appropriate materials and equipment needed for daily operations. At the end of winter quarter 2008 it was decided to redirect some funds to cover the costs of phase 2 of the BEP. Phase 2 of the BEP involved the installation of an appleseed style reactor and was originally planned to be budgeted for and installed fall quarter 2008. An appleseed reactor refers to a system that utilizes a standard home electric hot water heater as the primary vessel to convert waste cooking oil into biodiesel. This type of system is a vast improvement over the original reaction vessel; offering better temperature control, improved chemical resistance, and will reduce time necessary to produce biodiesel. Together with the wash tank, this setup should more than double the production capacity of the biodiesel processing facility. The only bad news is that it is likely that the supply of waste cooking oil coming from campus will not meet the demands of the processing facility operating at full capacity. Phase 2 of the BEP is complete. At the end of spring quarter 2008 the facility has produced 75 gallons of biodiesel in just 2 weeks.

SAFETY PROCEDURE
The following information contains excerpts from TESC Lab Safety Manual.ii Megan Ellis-Treasure modified this Edition March 2008. Please read the entire Lab Safety Manual and be familiar with it before proceeding. The Biodiesel Project Operators are responsible for obtaining any additional chemical fact sheets or safety information when operation modifications are made. (The Lab Safety Manual may be obtained from TESC Lab Stores or by downloading it from: http://scicomp.evergreen.edu/images/lab_safety_manual.pdf)

General Emergency Procedures:

Know the locations and proper use of each piece of emergency equipment in the biodiesel Production Facility and Lab space. This packet provides the knowledge of the following: Spill Kits Exits Eye Wash First Aid Kits Fire Extinguishers Telephones Personal Protective Equipment If an emergency occurs, the first concern is for the health and safety of people in the area; property damage is secondary. - Alert co-workers in the area of danger. - Assess the severity of the emergency. - Based upon the severity of the emergency, Call for Help. Telephone Locations 1. The blue emergency phone outside the farm workroom calls Police Services. 2. There is a phone inside the farm workroom that requires dialing 9 for any outside call. Dialing 9 is not required for calling campus extensions. Extreme Emergency McLane Fire Dept TESC Police Services Lab Stores 9-911 x6140 x6489 0-800-542-6319 Lab II, 1265 x6111 (8 am to 5 pm) Facilities x6120 (after hours) Steam Plant x6318

M-F, 8 am 5 pm Poison Center: Environmental Health and Safety: Building Maintenance Problems:

When reporting an emergency, give: Building, room number, or other location Nature of the emergency The number you are calling from Your name

Evacuate the area and keep people from re-entering before help arrives. IF UNSURE OF THE SEVERITY, CALL POLICE SERVICES ON THE BLUE EMERGENCY PHONE or X6140 FROM INSIDE THE WORK ROOM. Dont hesitate to ask for immediate help. Your health and safety are important! Do not attempt to move an unconscious person unless you know the nature of the emergency. MANDATORY LAB AND STUDIO RULES These rules apply to all individuals utilizing the science and art labs at The Evergreen State College. Violation of any of the following rules is cause for disciplinary action including forfeiture of laboratory use privileges. Everyone is responsible for complying with the safe practices and rules set forth in this manual in addition to complying with all legal regulations governing laboratory work and handling and disposal of chemicals and hazardous materials. If any of these rules are unclear, ask the lab staff for clarification. Shoes are required in the Biodiesel Facility and all Lab buildings at all times. Food and drink are prohibited in Biodiesel Facility and all lab rooms, including gum and chewing tobacco. Do not store food or beverages in the facilities. You or your food may be removed from the lab if this rule is not followed. Mouth pipetting is prohibited. Eye protection must be worn when doing chemical work and in chemical handling and storage areas. When there is a possibility of violent reaction, goggles, face shield or portable explosion shield must be used. Wearing contact lenses with goggles or face shields is not recommended. Closed-toed shoes and long pants or long skirts are required when working with chemicals. You must limit exposed skin as much as possible. If you wear inappropriate clothing for lab, you will not be allowed to participate. Lab coats and protective gloves as well as goggles, are recommended at all times when handling chemicals. Hair that is shoulder length or longer must be pulled back. Long, loose sleeves, jewelry, etc. must also be secured to prevent being caught or dragged. Wash hands thoroughly after working in the lab. Backpacks and coats should not be stored on lab tables or on the floor. Cubbies are provided for storage of personal items. In order to keep the cubbies clean, no chemicals, glassware, specimens, etc. may be stored in them. It is the responsibility of the individual using chemicals or equipment to know the associated hazards of each and to handle them accordingly. All chemical containers must be clearly labeled with contents, date, hazards and a HMIS rating label including the MSDS number (see Section IV-B and IV-C). When you transfer chemicals, label the new container with your name and date as well as the above information. FIRE PREVENTION Eliminating the source of ignition can prevent fires. When working with

flammable materials, consider all potential sources of ignition: open flames, sparks, electrical sparks from motors, etc. GENERAL - WHEN A FIRE OCCURS Prompt action may prevent small fires from getting out of control. Alert others in the area of the fire and send someone for help. Placing an inverted beaker or a watch glass over the fire can smother small fires in glassware. If the fire is too large to smother, evacuate the area. Only people trained in fire extinguisher use should attempt to fight the fire. NEVER ATTEMPT TO FIGHT A FIRE ALONE. When fighting a fire, put yourself between the fire and the exit to ensure a means of escape. If the fire can't be immediately controlled, call the fire department at 9-911. Pull the alarm located by the exits and stairways in each lab building. Try to contain the fire to the lab area by closing fume hood sashes, windows, and the doors to the lab as you leave. PEOPLE If clothing, skin, or hair catches fire, drop to the ground and roll to smother the flames. You may need to help push the person to the ground to prevent them from running and fanning the flames. Safety showers are in or near all lab rooms, and can also be used to put out a fire. Send someone to call for help, 9-911 METALS Metal fires cannot be extinguished with regular extinguishers. Use a Class D fire extinguisher or sand to smother the fire (CO2 and dry chemical extinguishers will intensify some types of metal fires). Before starting work with metals such as Sodium, Potassium, or powdered Aluminum or Magnesium, check that there is sand or a Class D fire extinguisher located in your area. CHEMICAL SPILLS Consider what to do in the event of a spill before starting a project. Spills may cause serious health and environmental problems if not handled correctly. Familiarity with chemical hazards and the proper spill control measures will help minimize the effects of a chemical spill. Again, the first concern is for the health and safety of the people in the area; property damage is secondary. CHEMICAL SPILLS, GENERAL PROCEDURES Immediately alert co-workers in the area of the danger. Assess the severity of the emergency. Consider the possibility of exposure through contact, inhalation, and the increased fire hazard associated with flammable materials. Based upon your best judgment of priorities, and knowledge of the chemical, Call for Help: Emergency McLane Fire Dept. M-F 8am to 5pm

Lab Stores

9-911 x6489

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Evenings and Weekends

Security

x6140 (0)

If necessary, you may need to pull the fire alarm, and/or evacuate the area and keep people from re-entering before help arrives. The person spilling the chemical is responsible for contacting lab staff/faculty as soon as the severity of the spill allows. Minor spills not involving human contact should be contained whenever possible. Depending on the hazard and size of the spill, lab staff/faculty will either direct the person responsible to clean up the spill or perform the clean up themselves. Anyone noticing a leak or spill is also responsible for contacting lab staff/faculty to initiate the clean up process. Spill kits are located in every lab room. These should be found in the lab reconnoiter exercise that accompanies the safety quiz. Before any chemical experiment begins, learn how to use the spill kits: that is, the proper absorbent and the proper neutralizer for the type of spill.

CLEAN-UP PROCEDURE
Methanol: - Turn off pump, heat strap and fan. - Open both doors to create a draft and leave the room. - Notify others in the vicinity. Methoxide: - Turn off pump, heat strap and fan. - Open both doors to create a draft and leave the room. - Notify others in the vicinity. - Cover the spilled area with bicarbonate from the caustic spill kit. - Scoop up with a plastic tool. - Place into a suitable container for disposal. Glycerin, Biodiesel, or Oil: - Apply kitty litter to soak up liquid. - Scoop up with a non-sparking tool. - Place into a suitable container. CHEMICAL SPILLS ON PEOPLE If a chemical is spilled on a person, IMMEDIATELY rinse the exposed area of the body and continue rinsing for 15 minutes. Use an eyewash station, emergency shower, or the sink to rinse the exposed area. Consult the MSDS for information on any delayed bodily reactions. Notify the person in charge to fill out an Accident Report. Eyes are extremely susceptible to chemical burns. Prompt and continued rinsing (for 15 minutes) can prevent severe eye damage. If your lab partner has a chemical splashed in their eye, you should assist them to the eyewash and ensure they rinse for the full 15 minutes, even if it is uncomfortable. Seek medical attention as soon as possible, and bring the MSDS with you to the emergency room or physicians office.

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In the event the spill contaminates clothing, remove all contaminated clothing and rinse the exposed area for 15 minutes. Extra clothing is available at Lab Stores. If the exposure is severe, someone in the area must call 9-911 to get paramedics on the scene. Be sure to continue rinsing the exposed areas until directed to stop by the paramedics. In the case of minor exposures: rinse affected areas for a minimum of 15 minutes, seek medical attention, and bring the MSDS with you.

FLAMMABLE MATERIALS If flammable materials have been spilled, immediately eliminate all sources of ignition. Unplug all electrical devices, extinguish open flames, etc. Absorb the material quickly with the appropriate spill absorbent, and call Lab Stores. CHEMICAL STORAGE Incompatible chemicals are chemicals that have potential for a violent reaction with each other (examples of specific incompatible chemicals are listed in Appendix 6). Hazardous chemicals (for storage definition) are chemicals with any HMIS category rating greater than 2. Methanol in the processing facility must be stored in the flame cabinet at all times. The flame cabinet can hold up to six 20-liter cans of methanol and a few other, smaller containers. Lye, is Incompatible with methanol and must not be stored in the flame cabinet. Lye is a corrosive and thus not compatible with flammable liquids stored in metal containers. General Guidelines: Date all chemicals when received and opened. Inventory annually, checking dates, condition, and amounts. Check particularly for ethers and peroxide forming materials, and discard within one year of opening. Avoid storing hazardous chemicals above eye level. Do not store chemical containers on the floor. Open shelves must have lips or doors to prevent bottles from slipping off. Any chemicals left unattended for ANY length of time must be stored in a closed container and properly labeled with name, date, program, chemical name(s), and concentration. Keep incompatible chemicals separated. Select an appropriate container (see Section IX-B and Appendix 7). Store away from heat and direct sunlight. Segregate bottles of chemicals in plastic tubs to contain any spill and maintain separation. For temporary storage, non-hazardous chemicals should be stored at the rear of a counter or in the center of an island. Hazardous chemicals are to be stored in a fume hood or vented cabinet.

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TRANSPORTING CHEMICALS The level of care and protection needed to transport a chemical must match the potential hazards of the chemical. This requires knowledge of the hazards associated with the chemical in transport and knowledge of protective measures. All chemicals must be placed in secondary containment while in transport. Acid buckets and plastic tubs are available from Lab Stores. Transport incompatible chemicals separately; place incompatible chemicals in separate carriers. All concentrated acids and bases must be carried in acid carriers. Use care when crossing the thresholds between the lab buildings. It is recommended to use the connecting basement level between Lab I and Lab II to avoid thresholds, extra doors, uneven surfaces and inclement weather. Do not ride the elevator when transporting volatile chemicals. Label the cart Do not ride with this elevator, send the cart up the elevator, and walk up the stairs to meet it. If the elevator breaks down, you do not want to be trapped in a small space with volatile and hazardous chemicals.

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CHEMICAL FACT SHEETS

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OPERATION PROCEDURE
In Biodiesel Facility: Always wear gloves, protective eyewear and appropriate clothing If cleaning, wear dust mask Close all valves Make sure the work area is tidy Retrieval and transit: WVO is currently collected from our 55 gallon barrel in the CAB. The steel barrel is labeled Fryer Oil Only and located under the WARNING sign. WVO is transported back to the Processing Facility in the 5 gallon plastic carboys that fryer oil is sold in. These jugs are commonly found in the recycling bin in the CAB and dirty ones should be replaced with fresh ones frequently. These jugs are also great to transport waste glycerin, wash water, biodiesel and oil to the leech-aid-tank where it is disposed. 1. 2. Load the hand pump and 5 gallon carboys into the back of the truck and secure with bungee cords. Bring a rag or 2 with you as you drive to the CAB. Once in the CAB, back the truck up onto the hydraulic lift until the rear bumper almost touches the rubber bumper on the wall. The control for the lift is to the right of the roll-up door. Raise or lower the bumper of the truck so that is level with the floor. If a barrel is being filled and transported, back up slowly until the bumper reaches the loading dock, so the dolly can role on to the bed of the truck easily with a heavy load. Slide the hand pump into the bunghole in the lid of the Fryer Oil Only barrel until it rests on the bottom of the barrel. Sludge, water and food parts, if present, will collect at the bottom of any WVO receptacle. If it is noticed that any of the above impurities are being pumped, hold the inlet of the pump 1 or 2 inches above the bottom of the barrel. And once empty, load barrel into truck, transport and clean the barrel with the pressure washer in next to Motor Pool. A piece of cardboard should be placed underneath the 5 gallon carboys when filling to catch any spilled oil. Cardboard can be found in the appropriate recycling bin in the CAB and can be disposed of after each use. Place the braded vinyl tubing end of the pump onto a clean 5 gallon plastic carboy: fill and cap. Repeat this step until all oil is removed from the Fryer Oil Only barrel. Place the full 5 gallon jugs on to the bed of the truck and secure with bungee cords. Place other materials in truck, clean up any spilled oil and drive back to the processing facility slowly Once back at the Processing Facility park the truck in front of the door. Unload the jugs and place on the floor or work bench. Move the truck in front of the work room, park and return keys.

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7. 8.

Now the WVO will be filtered. Pore the WVO from all 5 gallon jugs through mesh strainer placed over the plastic blue storage barrel. After WVO is filtered, back flush strainer with hose to the left of the back door. Hang strainer in processing facility where it can dry.

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Biodiesel Laboratory Manual

A lab safety class must be taken through Lab Stores prior to embarking on laboratory work. Once this class is completed then the Project Information and Approval form and Equipment/Chemical Request form must be filled out, signed by the current sponsor and returned to Lab Stores. In the past Room 2064 in Lab 1 has been used by the Evergreen Biodiesel Project. There should be a lab binder/notebook that remains in the lab for the duration of the quarter. Electronic lab notes and batch worksheet templates were created to make lab records more consistent and are saved on the BD manual disk. Chemicals should be stored in a chemical storage cabinet, under the hooded area in Lab 2064. It is always best to work at least one teammate in the Lab, though it is not required. Processes in the lab should parallel facility processes as closely as possible. Please record any observations or deviations from the following steps in the Lab notes. Updating the BD Manual at the end of each quarter will allow others to benefit from your trials and tribulations. THE EVERGREEN STATE COLLEGE LAB SAFETY PROCEDURES SHOULD BE FOLLOWED AT ALL TIMES!!!

Lab Equipment Master List Always use glass or metal equipment if it will contact chemicals plastic will deteriorate. All chemicals and substances should be labeled per lab safety procedures!
Protective eyewear Nitrile gloves, properly sized Lab coat or protective apron Lab binder/notebook and pen Labeling tape and marker 2-1500 mL beakers 2-500 mL beakers (600 mL Pyrex) 150 mL beaker 100 mL beaker 20 mL beaker 2 -100 mL graduated cylinders 2 2000 mL Separatory Funnels (conical with bottom valve) with stopcocks 2 Ring stands and with rings sized for separatory funnels Burette Burette stand and clamp Glass funnel

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Glass stir rod Blender (glass or metal) Stir plate 2- Stir magnets, small and large Magnet retrieval wand Scale Weighing paper Metal scoop for lye Syringe (5 cc or 5 mL) Thermometer Light Density Liquid Hydrometer (0.7 to 1.0) Phenolphthalein (small bottle) *Di-ionized water (DI) DI water carboy or other DI water vessel *Waste Vegetable Oil (WVO) from Organic Farm BD Facility should already be filtered *Isopropyl Alcohol *Methanol *Lye (KOH) Waste product container (for chemical waste such as glycerin)

*After reading through the manual you can estimate the amount of each chemical you will need for the quarter.

Titration:
Lab safety procedures should be observed for all Lab work. Fill out the Lab notes throughout the process. Titration determines the amount of catalyst needed for transesterification. A proper titration can result in a more complete reaction between the oil and alcohol. After experience is gained one titration will take 15-20 minutes. 1. First gather all non chemical required materials: Protective gear eyewear, apron and gloves Labeling tape and marker Lab Notes, Batch Worksheet and pen *100 mL beaker 20 mL beaker Stir plate Small magnet Magnet retrieval wand *Scale *Weigh paper *Metal scoop for lye

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Burette Burette stand Glass funnel Syringe (5 cc or 5 mL) *100 mL Di-ionized water (DI) 3 mL Waste Vegetable Oil (WVO) from Organic Farm BD Facility (filtered)

Verify that all required chemical amounts are present in lab. Chemicals that pose a safety hazard should be kept in the appropriate storage area until needed. Phenolphthalein 10 mL Isopropyl Alcohol *0.1 gram Lye (KOH) Waste product container

* Only required if there is not a solution of lye/DI prepared from a previous titration. 2. Put on personal protective gear and make sure the work area is tidy and all equipment is clean and dry. 3. Set up stir plate. Plug in under hood. 4. Set up the burette stand so that the burette is directly over the stir plate with enough space to put the 20 mL beaker underneath it. This should all be set up under the hood. 5. Measure 10 mL isopropyl alcohol into the 20 mL beaker. 6. Using the syringe measure 1 mL of WVO. Label syringe. Measuring exactly 1 mL is extremely difficult. Collect 3 mL in the syringe, though only 1 mL will be used. Leaving an air bubble on the plunger side of the syringe helps to accurately read the volume. 7. Add the 1 mL WVO to the 10 mL isopropyl alcohol and label per lab safety guidelines. 8. Place the 20 mL beaker onto the center of the stir plate and place small stir magnet inside beaker. Turn the stir plate onto 7. Let the WVO isopropyl alcohol mixture blend until there are no visible oil pockets.

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9. Determine the amount of lye and DI required for the volume of lye/DI solution you wish to make OR use previously prepared lye/DI solution. A 1:1000 ratio of lye to water is required. Typically use 0.1 grams lye to 100 mL DI. Remaining lye/DI solution may be stored in a tightly sealed container, labeled and used for future titrations. 10. Pour predetermined amount of DI (100 mL) into the 100 mL beaker. 11. Weigh out the predetermined amount of lye (0.1 g) using weigh paper, scale and metal scoop. 12. Add the lye to the DI. This is an exothermic reaction. The lye should dissolve fairly rapidly. Make sure the lye is completely dissolved into the water before proceeding. Label per lab safety guidelines. 13. Using the glass funnel, fill the burette up to a whole number measurement with the lye/DI solution. MAKE SURE THE BURETTE VALVE IS CLOSED BEFORE FILLING! Take a base line reading of the volume of lye/DI solution in the burette and record in the Lab Notes. Store remaining lye/DI solution in a sealed container with label per lab safety guidelines. 14. The burette stand should be situated above the 20 mL beaker on stir plate. Turn the stir plate down to 4. 15. Add five drops of phenolphthalein to the isopropyl/oil mixture (it should be a murky yellow color). 16. Start dripping lye/water solution into WVO/alcohol mixture. Drip very slowly, pausing to observe color changes. 17. Observe the color of the isopropyl/oil mixture. When a light pink (rose) color is sustained for 30 seconds you have reached the appropriate pH. Stop the drip when the light pink color is sustained for 30 seconds. If you are unsure take note of the suspected appropriate level and continue with the drip. If it turns purple you have gone too far.

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18. The amount of lye/DI solution needed to reach the optimal pH can be determined by subtracting the amount left in the burette from the original volume put into the burette. Typically around 3 mL of the lye/DI solution is used. 19. 1 mL of lye/water solution added is equal to 1 gram of lye per 1 liter oil. 20. X mL lye/water + 7 =grams of potassium hydroxide (KOH) needed per 1 liter WVO 21. Record the results in the Lab Notes and on the Batch Worksheet. 22. The batch worksheet can then be routed to the BD facility for use on a large batch. 23. Clean up while still wearing protective gear! RETRIEVE THE MAGNET FROM THE 20 ML BEAKER (IT WILL FIT DOWN THE DRAIN!). The contents of the 20 mL beaker may be poured down the drain (lye is a main ingredient in draino and isopropyl alcohol is similar to rubbing alcohol). The lye/DI solution may be stored in a sealed container, labeled per lab safety guidelines, in the chemical storage area under the hood. The titration results are specific to the WVO used in the test. When using oil from multiple collections the sample brought to the lab should be representative of the oil that will be used in the large batch. New titrations should be completed when any additional oil is added to the BD facilities oil. Completing titrations just prior to starting a large batch is the best way to ensure that the titration results are accurate and additional oil will not be collected.

Laboratory Small Batch

Lab safety procedures should be observed for all Lab work. Fill out the Lab notes throughout the process. Making a small laboratory batch is a great way to become familiar with the process of transesterification. Small batches can be used to test titration results that seem questionable and also to experiment with new methodologies.

Transesterification
Transesterification is the process in which biodiesel is created by reacting alcohol, methanol or ethanol, with oil in the presence of a catalyst, typically lye. After the transesterification the liquid needs to settle and separate into glycerin and biodiesel. The glycerin is removed and the biodiesel washed with water and allowed to dry.

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1.

First gather the non chemical required materials: Protective gear eyewear, apron and gloves Labeling tape and marker Lab Notes, Batch Worksheet and pen 1500 mL beaker 500 mL beaker Stir plate Large magnet Magnet retrieval wand Scale Weigh paper Metal scoop for lye 2000 mL separatory Funnel and stopcock Ring stand and ring sized for separatory funnel Thermometer Glass funnel Blender 1000 mL Waste Vegetable Oil (WVO) from Organic Farm BD Facility (filtered)

Verify that all required chemical amounts are present in lab. Chemicals that pose a safety hazard should be kept in the appropriate storage until needed. 200 mL Methanol Lye (KOH) determined through titration Waste product container

2. Put on personal protective gear and make sure the work area is tidy and all equipment is clean and dry. 3. Set up stir plate and blender. Plug in under hood. 4. Set up ring stand and a 2000 mL separatory funnel under the hood in close proximity to the stir plate. 5. Measure out 1000 mL of WVO into 1500 mL beaker and label per lab safety guidelines. 6. Place 1500 mL beaker of oil onto stir plate under hood. Gently drop in large stir magnet. Turn heat to 4. Turn stir plate to 7. Sustain temperature above 120 C until oil surface is glassy. This boils out any water in the oil. Water can hinder the reaction.

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Turn off and let cool.

7. Measure out 200 mL of methanol into 500 mL beaker. This should be done under the hood with careful attention to safety! Keep chemical container capped as much as possible to reduce fumes and water absorption. Methanol will absorb water from the air so work quickly. Pour into blender and put lid on. Leave under hood while you weigh out predetermined amount of lye. 8. Weigh out the predetermined amount of lye using the scale, weigh paper and metal scoop. Lye will also absorb water so again, do not leave it sitting out long and keep the lid on the chemical container as much as possible. Open the hood and remove blender lid prior to removing the weigh paper and lye from the scale. 9. Add the lye to the methanol in the blender, under the hood. Put lid on. Pulse the blender in 3 30 second intervals over the course of 5 minutes. Remove the lid and verify that the lye is dissolved into the methanol. DO NOT INHALE ANY FUMES FROM THE METHANOL!!! Tilt the blender towards yourself and look through the glass of the hood. This new mixture is called Potassium methoxide and is a poisonous chemical. DO NOT INHALE FUMES!!! This is an exothermic reaction so the blender container may be warm, use caution when handling. Label per lab safety guidelines. 10. Verify that oil is below 60 C. Methoxide has a low flash point and boiling point. 11. Add the Potassium methoxide to the oil and allow the mixture to stir for 15 minutes. Stir plate should still be on 7. Label per lab safety guidelines. Use this time to make observations, record deviations from manual and start to clean up. 12. Turn off stir plate and retrieve large magnet using the retrieval wand. Have an empty beaker on hand to put the dirty magnet in prior to washing. 13. Make sure the 1500 mL beaker is not hot.

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14. Remove stopcock from separatory funnel and place glass funnel inside. MAKE SURE THE SEPARATORY FUNNEL VALVE IS CLOSED BEFORE FILLING! Double check that the magnet has been removed from the 1500 mL beaker! 15. Pour mixture into separatory funnel and put on stopcock. Label per lab safety guidelines. 16. Leave the mixture to settle for at least 8 hours. 17. Clean up and prepare to return in a day or two. 18. Upon return make observations about the glycerin and BD layers 19. If the glycerin does not settle out, hypothesize why. Try a second test batch. 20. If the reaction was completed there will be a very distinct glycerin layer beneath amber colored BD. 21. Place a 500 mL beaker beneath the valve of the separatory funnel. 22. REMOVE STOPCOCK FROM SEPERATORY FUNNEL. 23. Open valve and drain glycerin layer slowly. After it appears you have drained all of the glycerin, close the valve and let the BD settle for a few minutes then drain the last accumulation. When this is complete the glycerin may be poured into the waste product container. 24. Perform any preliminary quality tests (see below) on the unwashed biodiesel. 25. Clean up while still wearing protective gear. 26. If desired, proceed to the wash and dry steps.

Wash and Dry

Lab safety procedures should be observed for all Lab work. Fill out the Lab notes throughout the process. Washing the biodiesel will remove impurities as the water trickles down through the BD and the impurities bind to the water. After the wash process the biodiesel is left to dry in a well ventilated area to allow evaporation

37

1.

First gather the required materials: Protective gear eyewear, apron and gloves Labeling tape and marker Lab Notes, Batch Worksheet and pen 500 mL DI Water pH indicator strips and accompanying color scale Biodiesel (BD) in separatory funnel 1500 mL beaker

2. Put on personal protective gear and make sure the work area is tidy and all equipment is clean and dry. 3. Take a base pH measurement of the BD and record in Lab Notes. The pH of unwashed biodiesel is typically slightly basic (~8). The BD should remain under the hood. 4. Pour DI water into the biodiesel, agitating slightly. Label per lab safety guidelines. Too much agitation will cause emulsion and take a week to settle. 5. Lower quality biodiesel will have more impurities and take longer to wash. Let settle until water has separated from BD. The first wash should be left overnight, but subsequent washes may take less than 20 minutes. Wash water will be milky with a distinctive white layer beneath the BD. The biodiesel should be a clear amber color. If the biodiesel is cloudy it may need to settle longer or washed again. 6. After settling is complete (time depends on wash number and initial quality) the wash water may be drained. 7. Place a 500 mL beaker below the separatory funnel. 8. REMOVE STOPCOCK FROM SEPERATORY FUNNEL. 9. Open valve and drain wash water slowly. After it appears you have drained the wash water, close the valve and let the BD settle for a 5-10 minutes and drain the last accumulation. Wash water is highly diluted and may be poured down the drain. 10. Measure the pH of the washed biodiesel and record in Lab Notes. 11. Repeat steps 4-10 until the wash water is clear and the pH is approximately neutral.

38

When making observations and recording pH in the Lab note be sure to indicate which wash it is (i.e. wash #2). Record on Batch Worksheet if this is a Facility batch sample.

12. After the biodiesel has been washed it is time to dry. 13. Place a 1500 mL beaker below the separatory funnel. Label per lab safety guidelines. 14. REMOVE STOPCOCK FROM SEPERATORY FUNNEL. 15. Open valve and drain biodiesel slowly. 16. Leave labeled 1500 mL beaker under hood to dry for at least 8 hours. Record observations in Lab notes and continue to dry or place in a labeled biodiesel container. 17. Clean up will still wearing protective gear. Quality Tests Quality tests can be made on lab batches or a sample of a facilities batch. If the tests are on a facilities batch sample, then record the findings on the Batch Worksheet that should have accompanied the sample from the BD Facility. Lab safety procedures should be observed for all Lab work. Fill out the Lab notes throughout the process.

pH test
If a wash has been performed, then this quality test has already been completed. The pH of unwashed biodiesel is typically above 8. The pH of washed biodiesel should be approximately neutral (7). Make sure that the pH indicator strips are either new or of good quality or else this test will be difficult and inconclusive. This test is best done with multiple people to gain a consensus of the color of pH indicator paper. 1. First gather the required materials: Protective gear eyewear, apron and gloves Labeling tape and marker Lab Notes, Batch Worksheet and pen Biodiesel pH indicator strips and accompanying color scale 2. Put on personal protective gear and make sure the work area is tidy and all equipment is clean and dry 3. Immerse the pH paper in the biodiesel.

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4. Remove paper and compare to the pH color scale with in 30 seconds. Determining the color match is subjective, so it is best done with a group for consensus. Record on the Lab Notes as well as the Batch Worksheet. 5. Clean up.

Specific Gravity Test

A hydrometer is used to measure specific gravity, calibrated with respect to water, it will float in the biodiesel and the surface point will read the density. The density of fuel relates to the viscosity of the fuel and if the specific gravity is over 0.900 g/cm then the reaction was incomplete; the fuel could cause damage to the engine, increase emissions, engine wear and injector choking. The specific gravity should read between 0.860 and 0.900 but is at highest quality at 0.880 at 60F and should always be significantly less viscous than the waste vegetable oil used.iv 1. First gather the required materials: Protective gear eyewear, apron and gloves Labeling tape and marker Lab Notes, Batch Worksheet and pen 100 mL graduated cylinder Hydrometer for light density fluids 80 mL biodiesel 2. Put on personal protective gear and make sure the work area is tidy and all equipment is clean and dry. 3. Poured biodiesel into graduated cylinder. Quantity is not important you just need enough to register a reading on the hydrometer. Label per lab safety guidelines. 4. Place hydrometer into biodiesel. Verify that the hydrometer is afloat. 5. Recorded the specific gravity measurement from the hydrometer at the surface level of the biodiesel. Read the hydrometer not the volume! Surface level of the biodiesel is at the lowest point in the meniscus (surface level curve). ASTM standards for BD are between 0.86 and 0.90. 0.885 is the average specific gravity for biodiesel. Record on the Lab Notes as well as the Batch Worksheet.

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6. Clean up. Biodiesel can be pour back into BD container.

3/27 Test
The 3/27 test is designed to observe the degree of conversion of oil to biodiesel. One part biodiesel is mixed with 9 parts methanol. Biodiesel is soluble in methanol and the triglyceride (fatty acids) that did not convert to biodiesel float to the bottom of the graduated cylinder, to be observed. There are also diglycerides and monoglycerides present if there are triglycerides, which makes this a comparison test rather than a quantitative test. 1. First gather the required non chemical materials: Protective gear eyewear, apron and gloves Labeling tape and marker Lab Notes, Batch Worksheet and pen 100 mL graduated cylinder 20 mL beaker Glass stir rod 10 mL biodiesel Verify that all required chemical amounts are present in lab. Chemicals that pose a safety hazard should be kept in the appropriate storage until needed. 90 mL methanol Waste product container

2. Put on personal protective gear and make sure the work area is tidy and all equipment is clean and dry. 3. Measure 10 mL of biodiesel in the 20 mL beaker. 4. Under the hood measure 90 mL methanol into graduated cylinder. 5. Pour in biodiesel and stir. 6. Allow to settle for 30 minutes and record observations in the Lab Notes. This test can serve as a great way to measure progress in your batches and give you a general idea of how complete you transesterification is. Record observations and results on the Lab Notes as well as the Batch Worksheet. 7. Clean up while still wearing protective gear.

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3/27 test mixture can be disposed of in the waste product container.

Cloud Point Test

Cloud point test verifies the temperature at which biodiesel will begin to gel and/or freeze. The lower the cloud point temperature, the lower temperatures that the biodiesel is operable and therefore the higher the quality. 1. First gather the required non chemical materials: Protective gear eyewear, apron and gloves Labeling tape and marker Lab Notes, Batch Worksheet and pen Freezer 100 mL beaker Thermometer 50 mL biodiesel 2. Put on personal protective gear and make sure the work area is tidy and all equipment is clean and dry. 3. Measure 50 mL of biodiesel in 100 mL beaker. 4. Place beaker in a freezer. 5. Every 2 minutes check for visual clouding. 6. When clouding is observed remove the beaker from the freezer and immediately determined the temperature. 7. Record observations and results on the Lab Notes as well as the Batch Worksheet.

8. Clean up.

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BIODIESEL PRODUCTION EQUIPMENT Reactor 1 is a modified 50 gallon electric water heater. The 100 liter marking on the Sight Tube is not shown in this photo. Important components are labeled below.

43

This Equipment is referred to as the Processor System. It includes Pump # 1, valves, fittings, clamps and vinyl tubing.

44

D: Drain WT: Wash Tank M: Potassium Methoxide W: WVO, Waste DT: Drying Tank C: Circulation ST: Sight Tube (?): Rarely needs to be shut

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BIODIESEL PRODUCTION PROCEDURES

In Biodiesel Facility: Always wear gloves, protective eyewear and appropriate clothing If cleaning, wear dust mask Close all appropriate valves Make sure the work area is tidy Assuming you have already collected and tested the WVO, you are now ready to begin production. Read all steps carefully before proceeding. Measuring WVO: When using the equipment during spring 2008 it was discovered that valves D, C and (?) were not closed much during the production process. Valve (?) needs to be closed very little and as of spring 2008 has only needed to be closed for maintenance reasons. 1. WVO will be measured and pumped into Reactor 1 for heating at this time. WVO is measured after pumping it from blue storage barrel into the Reactor and observing the oil level through the sight tube. The Sight tube is currently marked at 100 liters (26.4 gallons). Place the tube connected to valve W into blue Storage Barrel. Open valves W, (?) and C. All other valves must be closed. Turn on Pump # 1 and fill reactor with approximately 100 liters of WVO. To use the sight tube, turn off Pump # 1 and open valve ST. Make a precise measurement by filling Reactor 1 above the level marked on the sight tube and then slowly drain WVO until the level of WVO in the sight tube matches the marking. Sight WVO level with the uppermost portion of the 100 liter marking on the sight tube. Once desired level is reached lift the tube connected to valve W from the oil in the storage barrel and let the pump evacuate the oil from the tubing for a few seconds before shutting off Pump # 1. Clean up any spilled WVO before proceeding to the next step.

2. 3. 4. 5.

6.

7.

Heating: 1. 2. With the processor filled with the appropriate amount of WVO, the heating element can be turned on. The thermostat inside Reactor 1 is set to 120 degrees Fahrenheit, but it measures the temperature of the oil at the level of the heating element, which is about 6 inches from the bottom of the tank. Thus the oil above the heating element can become hotter than 120 degrees. To avoid overheating, open Valves D, (?) and C, turn on Pump # 1 and circulate the WVO for 5 or 10 minuets before turning off

46

3.

the pump and closing valves D and C. This step should be performed about once an hour until transesterification begins. One may expect heating a 100 liter batch to take 5 or more hours.

Potassium Methoxide Prep: Important: Avoid inhaling all fumes from the methanol, or the dust from the lye. Lye is a corrosive and should not be stored in the flame cabinet. In this document lye refers to potassium hydroxide also known as KOH. It is illegal to store methanol outside of the flame cabinet. The flame cabinet can hold 6, 20-liter cans of methanol. Once Potassium Methoxide is mixed and pumped into Reactor 1, the can must be disposed of. Dispose of the can by transporting it to lab immediately after use. Once in lab, place container in fume hood, label and uncap. Allow methanol to evaporate completely, then rinse out lye with lots of water before disposing in dumpster. One of the future goals of the Evergreen Biodiesel Project is to develop an improved technique for making potassium methoxide.

1.

2. 3. 4. 5. 6.

7.

8. 9.

In Lab: Measure the calculated amount of lye into 3 kg containers marked Storage and Transport; cap tightly. Place sealed container of lye into plastic tub and clean up work area. Then fill the green Potassium Methoxide Tub with a few inches of ice. Transport Lye and green Potassium Methoxide Tub to the processing facility. In Processing Facility: Turn on exhaust fan. You must wear protective eyewear, gloves, a chemical mask or hood, and BD suitable clothing: potassium methoxide is very dangerous. Remove methanol container from flame cabinet, and place in green Potassium Methoxide Tub with ice. Add 1 gallon of water to the ice in the Potassium Methoxide Tub. The water and ice bath will remove heat created by the exothermic reaction of lye dissolving in methanol. Uncap the methanol container and pour pre-measured lye directly into the container using a funnel made from a piece of paper. Do this step as quickly and safely as possible. The container and chemicals with in are now referred to as the Potassium Methoxide container and Potassium Methoxide respectively. Tightly cap the container and dispose of the funnel. Gently rock the container back and forth for 5 minutes to dissolve the lye. Let the chemicals sit for 10 minutes and then repeat this step 4 times, or until lye is completely dissolved. Mixing lye and methanol creates heat and gas. To be sure the Potassium Methoxide container doesnt build up excessive pressure; vent the container every few minuets by unscrewing the cap until pressure is released.

Transesterfication: The 50 gallon electric water heater currently used as Reactor 1 has been setup to process

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100 liters or 26.4 gallon of WVO at a time. Important: Do not attempt to transesterify any more than 35 gallons or less than 20 gallons of WVO in Reactor 1 at one time. The Heating Element must be turned off when any amount of fluid is removed from Reactor 1. The heating element in Reactor 1 is a 4500 watt stainless steel coil operating at 240 volts. If the heating element is turned on when it isnt well submerged it will burn out in just a few seconds and may cause fire. If a significant leak or problem is found in Reactor 1 or the processing system, the heating element must be turned off. To avoid air being sucked into the pump, the valve labeled ST should be closed any time Pump # 1 is on. Make measurements using the Sight Tube when Pump # 1 is off and Valve ST is open. 1. 2. Uncap Potassium Methoxide container and insert the tube connected to valve M until it reaches the bottom of the container. Open valves M, (?) and C and turn on Pump # 1. Once all the Potassium Methoxde is drained from its container, let the pump evacuate the tubing for a few seconds before switching it off. Close valve M and remove tube from Potassium Methoxide container. Tightly cap the empty Potassium Methoxide container and place back into green Potassium Methoxide tub after emptying ice and water. Have a team member transport Potassium Methoxide container and tub to your Lab room immediately. The residual chemicals in the container will continue to build pressure. Dispose of Potassium Methoxide container as described in Potassium Methoxide Prep. Section and return Potassium Methoxide tub to the processing facility. Open valve D and turn on Pump # 1. The pump will mix the WVO and Potassium Methoxide to create biodiesel and glycerin. The pump needs to mix the ingredients for one and a half hours to ensure proper separation. Batches larger than 100 liters should be mixed longer. After transesterification is complete, turn off Pump # 1, the Heating Element and close valve C. Open valve WT and place the tube connected to valve WT into the appropriate wash tank. Turn on Pump # 1 and transfer the biodiesel and glycerin in Reactor 1 to the wash tank for settling. Once Reactor 1 is empty, let the pump cycle for a few seconds to evacuate the tubing before turning it off. Close valve WT and return the tubing connected to valve WT to its proper place.

3. 4.

5.

6. 7. 8.

9.

Draining Glycerin: All waste glycerin, waste wash water and waste biodiesel should be transported and disposed of the same day it is created. This waste is to be disposed of in the leech-aidtank behind compost bays 2 and 3. Once waste is dumped, rinse all surfaces in the leechaid-tank that came into contact with the waste with water from the compost hose. If it is observed that the tank is nearing capacity notify Melissa Barker or Alex Morow so that it can be pumped and hauled away as needed.

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1. 2. 3.

4.

Allow biodiesel and glycerin to settle for 48 hours before draining glycerin. Place the tube connected to the valve labeled Drain on the appropriate wash tank into a bucket or 5 gallon plastic carboy. Open the valve labeled Drain to allow glycerin to flow into the container. Once container is almost full close valve W, move the tube connected to valve W to an empty container and fill: Repeat this step until a small amount of biodiesel begins to flow through the tubing. Transport glycerin to leech-aid-tank, dump and rinse tank. At this point more glycerin can be drained from biodiesel if let to settle: there will always be more glycerin settling from the biodiesel. The biodiesel in Reactor 1 is now ready to be washed: Any remaining glycerin will have time to settle during the washing process.

Washing There are currently two wash tanks in the biodiesel processing facility, a 55 gallon conical bottom polyethylene tank and a modified 55 gallon steel barrel which once was the facilities main reactor. These wash tanks are labeled Wash Tank 1 and Wash Tank 2 respectively. Wash Tank 1 is currently outfitted with a more advanced bubble wash compared to Wash Tank 2, which uses a mist washer. Wash Tank 1 should be used when ever possible. The procedures for washing biodiesel differ slightly between wash tanks 1 and 2 and are detailed in separate sections below. Each batch of biodiesel should be washed 3 times. After each wash the pH of biodiesel should be measured with pH strips. The pH of biodiesel should become closer to neutral as washing removes residual lye. After the third wash the biodiesel should be near neutral pH. Wash Tank 1: 1. For a 100 liter batch, fill Wash Tank 1 with about 10 gallons of water from the faucet to the left of the back door. The water should be let into the tank such that there is minimal mixing of wash water and biodiesel. Measure and record the pH of the biodiesel at this point. The pH of unwashed biodiesel should be between 8 and 10 Place the diffuser into the Wash Tank making sure it well submerged in the water. Turn on the air pump and let the bubbles wash the biodiesel for about 10 minuets. After turning off the air pump, the biodiesel and wash water must be left to settle for at least 24 hours before draining the waste wash water. After settling place, the tube connected to the Drain valve on Wash Tank 1 into a 5 gallon plastic carboy, open the Drain valve and fill carboy. Repeat this step until all waste wash water is drained from Wash Tank 1 into 5 gallon carboys. Stop draining when the water becomes murky and the viscosity changes (from thin water to thicker biodiesel). Let wash water settle for some time and then drain remaining wash water. Transport the waste wash water to the leech-aid-tank and dispose of as described above.

2. 3. 4. 5. 6.

7. 8.

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9.

Repeat steps 1 through 8 two more times so that the biodiesel is washed a total of 3 times. With each successive wash increase the length of time the biodiesel and water are mixed by the air pump. The second time biodiesel is washed leave the air pump on for 30 minuets and the third time for an hour. This will reduce the chances of forming an emulsion. Measure and record the pH of each batch of waste wash water before disposal.

Wash Tank 2: 10. Place mister in lid and turn on the faucet to the left of the back door. Check for leaks and then turn on the mister. Keep acute attention on the water level at all times. Fill Wash Tank 2 until there is a quarter to a third the amount of water to biodiesel. The biodiesel level will rise as water goes in. Turn off water and detach hose. Allow the biodiesel and wash water to settle for at least 24 hours before draining the waste wash water. Place the tube connected to the valve labeled Drain on Wash Tank 2 into a 5 gallon plastic carboy. Open the valve labeled Drain on Wash Tank 2 and drain waste wash water into 5 gallon plastic carboys. Stop draining when the water becomes murky and the viscosity changes (from thin water to thicker biodiesel). Measure the pH of the wastewater and document it. Try not to open the lid of Wash Tank 2 at any time during this procedure because methanol will be evaporating. Repeat steps 10 through 14 two more times so that the biodiesel is washed a total of 3 times. Measure and record the pH of each batch of waste wash water before disposal.

11. 12. 13. 14.

15.

Drying: Biodiesel coming form the wash tank(s) that is cloudy likely appears this way because water is suspended in it. It was decided to build a Drying Tank one winter while making biodiesel when it took two weeks for a batch to dry (become clear) in an open container. The drying tank warms the biodiesel and aerates it to efficiently remove water. The drying tank was once the facilities storage tank and the orignal lid can be found hanging on the wall. Read the maintaince manual section titled: Tempco Silicone Rubber Drum Heater for manufactures information on the drying tank heaters before use. 1. Connect the tube connected to valve W to the wash tank from which biodiesel will be pumped to the drying tank. Open valves W, DT, (?) and the valve labeled Outlet on the bottom of the wash tank. Turn on Pump # 1 and drain the biodiesel into the Drying Tank. Once all the biodiesel is drained from the Wash Tank let the pump cycle for a few

2. 3.

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4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

seconds to evacuate the tube before switching off Pump # 1. Close valves W, DT and return the tube connected to valve W to its appropriate place. Flip the switch labeled Heat Belt on the wall to the ON position, and turn the heat belt thermostat(s) on the Drying Tank to no higher than 8. Warm biodiesel. A lid can be placed over the tank while heating, before Pump # 2 is turned on to circulate the biodiesel. Once biodiesel is warm remove the lid, open the valve labeled Drain on the Drying Tank and turn on Pump # 2. Circulate biodiesel for 1 to 2 hours. Turn off Pump # 2 and close the valve labeled Drain. Let the biodiesel settle for 15 minuets and observe clarity, much of the methanol has evaporated by now. If no further drying is needed, turn off the switch labeled Heat Belt and turn the heat belt thermostat(s) to 0. The biodiesel is now ready to be pumped into the Storage Tank. The Drying Tank should have a lid placed over it when it is not in use so dust does not collect inside it.

Storage: 1. To pump finished biodiesel in to the Storage Tank open valve ST, the valve labeled Drain on the Drying Tank, and turn on Pump # 2. 2. The drying Tank can be tipped when there are just a few gallons of biodiesel remaining inside it. This will maximize the amount of biodiesel transported to the Storage Tank. 3. Once all the biodiesel is pumped from the Drying Tank allow the pump to evacuate the tubing for a few seconds before switching off Pump # 2 and closing valve ST and the valve labeled Drain on the Drying Tank. 4. The fuel can now be dispensed from the Storage Tank into the yellow 5 gallon plastic fuel cans. When biodiesel is available, please keep the tool room stocked with B-100 or B-50 during cold weather.

Example of Catalyst Conversions

This section was created by the original biodiesel team and describes the amount of lye needed to transesterify a batch of biodiesel. The original biodiesel team believed that the quality of WVO coming from campus was consistent enough to not require titrations or test batches before each reaction. This chart says to use 7.5 grams of lye per liter of WVO. WVO in Gallons 20 21 22 KOH in Grams
568 596.4 624.8 WVO in Gallons 20 21 22 Methanol in Gallons 4 4.2 4.4

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23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50

653.2 681.6 710 738.4 766.8 795.2 823.6 852 880.4 908.8 937.2 965.6 994 1022.4 1050.8 1079.2 1107.6 1136 1164.4 1192.8 1221.2 1249.6 1278 1306.4 1334.8 1363.2 1391.6 1420

23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 10

4.6 4.8 5 5.2 5.4 5.6 5.8 6 6.2 6.4 6.6 6.8 7 7.2 7.4 7.6 7.8 8 8.2 8.4 8.6 8.8 9 9.2 9.4 9.6 9.8

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MAINTENANCE MANUAL
The equipment in the biodiesel processing facility has been well researched and should provide years of reliable service. However, as with any mechanical system, regular maintenance and inspection will ensure safety and reliability when using the equipment. Please follow the guidelines below and use common sense when inspecting and doing maintenance on the equipment. Pump # 1: Pump # 1 may become clogged with debris from the WVO at some point. If Pump # 1 seems to lose some of its power, it is likely that debris has collected at the inlet of the pump. Remove debris by removing the union near valve (?), then the piping and fittings from the inlet. Remove debris and reinstall components with fresh Teflon tape on the threads. Because the threads in Pump # 1 are not tapered, the two, 1-inch reducers on the pump require extra thread tape. Please refer to the manufacture information below for further information. Vinyl Tubing: The vinyl tubing in the processing facility will need to be replaced over time. When tubing becomes soft or loses its clear color it may need to be replaced. The tubing connected to valves C and M will likely need to be replaced more frequently than other tubing. Leaks: There are many threaded fittings on the current equipment in the processing facility, some of these will eventually leak. Inspect all threaded fittings for leaks on a regular basis. Slow leaks can simply be wiped up with a rag before using the equipment. For larger leaks; remove the affected parts, reapply generous amounts of thread tape and reinstall. If possible, tighten the leaking parts more than they were when leaking.

Manufactures Information:

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54

55

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RESOURCES
HUMAN RESOURCES
Should students require technical advice during any phases of the BEP, a short list of people to contact follows: Melissa Barker: Organic farm Manager. 360-867-6160 Melissa helped build the facility and is aware of nearly all activities that have occurred during the existence of Evergreen Biodiesel Project. Because the Evergreen Biodiesel Project is part of the Organic Farm, limited funding for things like lye and methanol can be secured through the Farm Budget. (These funds are VERY limited! You must apply for GRANTS)! Marty Beagle: Arts and Sciences Operation Manager. beaglem@evergreen.edu, 360-867-6466 Marty was involved with the construction of the biodiesel facility. He is very knowledgeable when it comes to construction, electrical and engineering projects. Marty maybe a good person to go to when it is found that you need a specific tool or a task accomplished that you are not prepared for (i.e. bolting equipment to the concrete). Michelle Bartlett: Fiscal Specialist. bartletm@evergreen.edu, 360-867-6484 Michelle is The Biodiesel Projects Budget Contact. Any equipment purchases need to be run through her. All receipts are given to Michelle for budgeting purposes. She is very helpful and fairly easy to contact.

EMERGENCY CONTACTS
See Biodiesel Safety Procedure (at the beginning of this document) for further contacts and safety precautions. McLane fire Dept: TESC Police Services (also Evening & Weekend contact): Lab Stores: 9-911 x6140 x6489

BIODIESEL RESOURCES
www.biodiesel.org www.biodieselcommunity.org www.attra.org www.evergreen.edu/cell/biodiesel www.ucsusa.org - union of concerned scientists www.veggiepower.org www.biodieselwarehouse.com www.gordosales.com/biodiesel www.journeytoforever.org

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CREDITS
All information in this manual (unless otherwise noted) was written by the Biodiesel Project Operators, Megan P. Ellis-Treasure and John Kemp, and by Sara Keehfuss. Megan and John would like to thank everyone that has been involved in the Evergreen Biodiesel Project throughout its existence.

BIBOLIOGRAPHY
Anonymous. The Evergreen Biodiesel Project. The Evergreen State College. Updated May 30, 2007. The Evergreen State College. Accessed February 12, 2008. <www.evergreen.edu/cell/Biodiesel.htm>.
ii i

Lab Stores. The Chemistry Club. Updated November 6, 2007. The Evergreen State College. February 12, 2008. <http://chemclub.evergreen.edu/science-support/labstores/> http://scicomp.evergreen.edu/images/lab_safety_manual.pdf.
iii

Chemtrec. Methly Alcohol. Updated August 10, 2004. MSDSonline. Mallinckrodt Chemicals and J.T. Baker. Accessed March 9, 2008. <http://www.msdsonline.com/>. Chemtrec. Potassium Hydroxide. Updated February 1, 2007. MSDSonline. Mallinckrodt Chemicals and J.T. Baker. Accessed March 9, 2008. http://www.msdsonline.com/.
iv

Tickell, Joshua; Tickell, Kia. From the Fryer to the Fuel Tank: The Complete Guide to Using Vegetable Oil as an Alternative Fuel. Tickell Energy Consulting. July 2000.

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