Quality System Procedure 08.4 Final Inspection for Marketers rev-08a00 / issued 11-07-08 - Approved by: Andy Erikson 1.0 Purpose and Scope The purpose of this procedure is to provide instructions, and to assign responsibility for performing and recording verification of final product and storage tanks. This procedure applies to all finished biodiesel and biodiesel blend products prior to shipping (and in some cases during shipping). This procedure applies to BQ-9000 Certified Marketers. 1.1 Definitions 1.1.1 ASTM: ASTM International, originally known as the American Society for Testing and Materials (ASTM), was formed over a century ago. ASTM International is one of the largest voluntary standards development organizations in the world. ASTM develops technical standards for materials, products, systems, and services. 1.1.2 Biodiesel: a fuel comprised of mono-alkyl esters of long chain fatty acids derived from vegetable oils or animal fats and meets ASTM D 6751, designated B100. 1.1.3 Blend: a blend of Biodiesel with fuel oils in a specified ratio, designated Bxx, where xx is the volume percent biodiesel. 1.1.4 External Lab: A third party laboratory that the biodiesel organization can use to test product samples. 1.1.5 Internal Laboratory: A laboratory that is operated or managed by the biodiesel organization. 1.1.6 Marketer: an entity engaged in the business of the distribution and sale of biodiesel and/or biodiesel blends of B2 or greater. 1.1.7 Producer: the entity responsible to the first purchaser of neat biodiesel for that neat biodiesel to meet the specification of ASTM D6751. A producer can also be engaged in the distribution of biodiesel blends of B99 or higher. 1.1.8 Verification: confirmation by examination and provision of objective evidence that specified requirements have been fulfilled. 08.4_08a00 UNCONTROLLED IF PRINTED page 1 of 6 Quality System Procedure 08.4 Final Inspection for Marketers rev-08a00 / issued 11-07-08 - Approved by: Andy Erikson 1.2 Discussion Formal ASTM biodiesel blends specification now include B1-B5, B6-B20, with variations for burner and fuel use. Associated regulatory controls exist. Compliance is critical. a) b) c) d) Retail Pump Labeling define fuel grades associated with regulatory controls (B1-B5,B6-B20,Bxx) ASTM D975 - diesel fuel may contain up to 5% biodiesel (B1-B5) ASTM D396 - fuel oils (burner, bioheat) may contain up to 5% biodiesel (B1-B5) ASTM D7267 – biodiesel blend specification for B6-B20 All finished products are subjected to final inspection before they are shipped. The Quality Assurance department is responsible for final inspections and for the release of product for shipping. This includes controls of final product lots within distribution tanks, and the verification of product at time of shipping. Storage tanks with inactivity are verified for continued quality of tank and product. The primary focus is on defect prevention, rather than detection. Normally, by the time products are completed they have been completely verified through the program of receiving and inprocess inspections. The purpose of final inspection is not to re-inspect the products, but to ascertain that all verification activities have indeed been carried out with satisfactory results. However, should there be suspect product nonconformance, the product is isolated and will not be shipped until corrective actions have been successfully completed. 2.0 Procedure 2.1 Method of Sampling ASTM D 4057, provides standard sampling methods. 2.2 Required Sample Volumes and Containers Reference WI 20-10-0001(Providing Samples to QA) for appropriate containers, identification, and volumes of fuels required for testing. 2.3 Nonconforming Product Procedures for Non-conforming product (QSP_09.1), define the actions required if product lot fails to pass required inspections or test. 2.4 Inspection Records QA Inspection Sheets log the inspection results, which includes product tested, appropriate traceability-ids, properties to test, property specification(acceptance limits), actual results, approval sign-off / date, test method specification, and test method revision. 08.4_08a00 UNCONTROLLED IF PRINTED page 2 of 6 Quality System Procedure 08.4 Final Inspection for Marketers rev-08a00 / issued 11-07-08 - Approved by: Andy Erikson 2.5 B100 Storage 2.5.1 B100 Storage & Distribution Tanks All B100 storage and distribution tanks should be dedicated to biodiesel service. If a tank is changed from some other service to biodiesel storage, the tank should be drained dry, cleaned, and then inspected. Inspection shall be documented. 2.5.2 B100 Storage Tank Sampling & Testing Quality assurance shall verify sustain quality of stored B100. Given the verification of B100 specification on receipt, verification is focused on the sustained quality of stored and aging fuel. B100 shall conform to ASTM D6751 specification. If out-of-specification, appropriate procedures are invoked: a) nonconforming product (QSP_09.1) b) corrective actions (QSP_10.1) 2.5.3 B100 Storage Tank Homogeneity Upper, middle and lower samples shall be taken every 30 days based on ASTM D 4057 sampling guidelines. All three samples shall conform to tank homogeneity requirements ASTM D 1298 or ASTM D 4052. If requirements are met, then a composite sample is created by combining the three upper, middle and lower samples for testing purposes in section 2.4.4 B100 Tank Testing. If relate density of samples fall outside the homogeneity requirements, then each sample must be tested individually. Property Relative Density Test Method Limits_________ ASTM D1298 or ASTM D4052 range 0.006 2.5.4 B100 Tank Testing Composite sample or individual upper, middle, lower sample, as determined by section 2.4.3, shall taken every 30 days and tested using the following: Property Flash Point, C-degrees Acid Number, mg KOH/gm Free Glycerin, % mass Total Glycerin, % mass Visual appearance Test Method ASTM D 6751 ASTM D 6751 ASTM D 6751 ASTM D 6751 ASTM D 4176(procedure 2) Limits_________ ASTM D 6751 ASTM D 6751 ASTM D 6751 ASTM D 6751 2 max If out-of-specification, appropriate procedures are invoked: c) nonconforming product (QSP_09.1) d) corrective actions (QSP_10.1) 2.5.5 B100 Product Distribution Samples If biodiesel is sold or distributed as B100 directly from a storage tank, a representative sample of product being loaded shall be retained for a minimum of 60 days. 08.4_08a00 UNCONTROLLED IF PRINTED page 3 of 6 Quality System Procedure 08.4 Final Inspection for Marketers rev-08a00 / issued 11-07-08 - Approved by: Andy Erikson 2.6 Fuel Blending and Distribution 2.6.1 Fuel Blending Fuels shall be blended and inspected per applicable blend specification and sales requirement. See referenced specification by B1-B5(road & bioheat), B6-B20. Fuel blending is a controlled process, which shall be performed and documented to ensure biodiesel blends are of correct product proportions and have been adequate mixed. This includes the measuring and recording the volumes and blend levels as verified through bills of lading, meter printouts, %blend inspection devices, or other auditable records of both the biodiesel and fuel oils which comprises the blend. These records shall be retained for a minimum of two years. 2.6.2 Blended Tank & Truck Homogeneity The process for blending biodiesel and fuel oils is validated for tank homogeneity after 5 consecutive blended lots meeting Tank Homogeneity requirements. To validate, the upper, middle and lower samples shall be taken based on ASTM D 4057 sampling guidelines. All three samples shall conform to tank homogeneity requirements: Property Relative Density Test Method ASTM D1298 or ASTM D4052 Limits_________ range 0.006 If operational parameters fall outside of the Tank Homogeneity requirements, the blend procedure shall be re-evaluated and revised as appropriate. Actions are documented per Corrective Action (QSP_10.1). 2.6.3 Tanks Containing Blended Biodiesel All blend tanks should be dedicated to biodiesel blend service. If a tank is changed from some other service to biodiesel blend storage or distribution, the tank should be drained and cleaned prior to use. Inspections shall be documented per Corrective and Preventive Action (QSP_10.1). Each time blending of biodiesel occurs, a composite sample of the blended fuel tank shall be obtained and retained for a minimum of 60 days. 2.6.4 Blended Fuel Tank Testing Blend tanks with no activity over a 30 day period shall be validated prior to use. An outlet sample shall be tested for moisture and sediment per ASTM D 4176 (procedure 2). If out-of-specification, appropriate procedures are invoked: a) nonconforming product (QSP_09.1) b) corrective actions (QSP_10.1) 2.6.5 Trucks or Tanks containing Blended Biodiesel 08.4_08a00 UNCONTROLLED IF PRINTED page 4 of 6 Quality System Procedure 08.4 Final Inspection for Marketers rev-08a00 / issued 11-07-08 - Approved by: Andy Erikson Each compartment of a truck, railcar or other vessel, shall be inspected to assure cleanliness and compatibility of previous load, prior to loading biodiesel product. If previous load contained a product that would contaminate the biodiesel or biodiesel blend product (e.g. gasoline, ethanol, methanol, lube oils, raw vegetable oil, animal fats, dyed product, ..), then affected compartments shall be drained, outlet line drained, and compartments verified for cleanliness prior to use. Contaminate list includes dyed product and products with excess of 15 ppm sulfur, when biodiesel or biodiesel blends are destined for ULSD applications. Any detected non-conformance shall be reported to the supervisor for appropriate corrective action per QSP_10.1 and equipment non-conformance reporting per QSP_9.1. 2.6.6 Transport Contracts Agreements and/or contracts with transport companies for truck rail and vessel shall state, explicitly or by reference, the cleanliness standards that shall be complied with before hauling. Periodic inspections shall be performed to verify transport company compliance with cleanliness specification. Any detected non-conformance shall be reported to the supervisor for appropriate corrective action per QSP_10.1 and equipment non-conformance reporting per QSP_9.1. 2.6.7 Product Distribution Samples ( Biodiesel Blends) A representative of sample product being loaded shall be obtained and retained for a minimum of 60 days. 3.0 Responsibilities Quality Assurance performs all the required inspections. Additionally, Quality Assurance establishes and maintains all appropriate inspection records and files. 4.0 References 4.1 Normative References - The following reference contains provisions which through reference in this text, constitute provisions of the procedure. References which are subject to revision shall always be used in the most recent form. BQ-9000 Quality Management System - Marketer Requirements ASTM D6751 Standard Specification for Biodiesel Fuel(B100) Blend Stock for Distillate Fuels ASTM D396 Standard Specification for Fuel Oils ( B1-B5) … bioheat / burners ASTM D975 Standard Specification for Diesel Fuel Oils ( B1-B5) ASTM D7467 Standard Specification for Diesel Fuel Oil, Biodiesel Blend (B6 to B20) ASTM D4057 Standard Practices for Manual Sampling of Petroleum and Petroleum Products 08.4_08a00 UNCONTROLLED IF PRINTED page 5 of 6 Quality System Procedure 08.4 Final Inspection for Marketers rev-08a00 / issued 11-07-08 - Approved by: Andy Erikson ASTM D1298 Standard Test Method for density, relative density ( Specific Gravity), or API Gravity Crude Petroleum and Liquid Petroleum Products by Hydrometer Method ASTM D4052 Standard Test Method for Density and relative density of Liquids by Digital Density Meter ASTM D4176 Standard Test Method for Free Water and Particulate Contamination in Distillate Fuels ( Visual Inspection Procedure ) QM QM 08.0 - Inspection & Testing 05.0 - Control of Quality Records QSP 09.1 - Control of Nonconforming Product QSP 10.0 - Corrective and Preventive Actions WI 20-10-0001 Providing Samples to QA 4.2 Informative References - The following references are included as bibliographic information, which may contain material useful in the execution of this procedure. References, which are subject to revision, shall always be used in the most recent form. BQ-9000 Quality Management System – Marketer Requirements WI 10-10-0001 QCS - Access to Online Quality Control System WI 10-10-0901 QCS - Nonconforming Product WI 10-10-1001 QCS - Corrective & Preventive Action Process Figure – 20-88-0001 Method of Inspection Table 4.3 Documentation/Records – The implementation of this procedure may require the use of the below listed forms and/or systems. QCS – Quality Control Solution ( online system ) Form_xx-xx-xxxx - Product Specification Sheets Form_xx-xx-xxxx - Certification of Analysis (COA) and other inspections Form_xx-xx-xxxx - QA Inspection Sheets 08.4_08a00 UNCONTROLLED IF PRINTED page 6 of 6